# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H48 N4 Pt2 S2' _chemical_formula_weight 895.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.525(3) _cell_length_b 15.830(5) _cell_length_c 11.853(4) _cell_angle_alpha 90.00 _cell_angle_beta 118.167(10) _cell_angle_gamma 90.00 _cell_volume 1575.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 110 _cell_measurement_reflns_used 9978 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 34.32 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 9.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3867 _exptl_absorpt_correction_T_max 0.5707 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa Axis Apex2' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32035 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 35.07 _reflns_number_total 5890 _reflns_number_gt 4884 _reflns_threshold_expression >2sigma(I) _computing_data_collection Apex2 _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution XS _computing_structure_refinement XL _computing_molecular_graphics NRCVAX _computing_publication_material cif2tables.py _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0130P)^2^+0.0504P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5890 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0399 _refine_ls_wR_factor_gt 0.0377 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 1.055086(9) 0.468543(5) 0.377457(7) 0.01109(3) Uani 1 1 d . . . S1 S 0.93466(6) 0.40590(3) 0.49891(5) 0.01360(11) Uani 1 1 d . . . N1 N 0.8270(2) 0.49702(11) 0.21705(17) 0.0133(4) Uani 1 1 d . . . C1 C 1.0590(3) 0.35653(13) 0.2879(2) 0.0182(5) Uani 1 1 d . . . H1A H 0.9827 0.3600 0.1966 0.027 Uiso 1 1 calc R . . H1B H 1.0301 0.3095 0.3265 0.027 Uiso 1 1 calc R . . H1C H 1.1662 0.3472 0.2983 0.027 Uiso 1 1 calc R . . C2 C 1.2873(3) 0.44347(14) 0.5102(2) 0.0175(5) Uani 1 1 d . . . H2A H 1.3412 0.4145 0.4683 0.026 Uiso 1 1 calc R . . H2B H 1.2889 0.4074 0.5779 0.026 Uiso 1 1 calc R . . H2C H 1.3425 0.4966 0.5475 0.026 Uiso 1 1 calc R . . C3 C 1.1259(3) 0.53204(13) 0.2653(2) 0.0153(4) Uani 1 1 d . . . C4 C 0.9972(3) 0.56112(14) 0.1507(2) 0.0155(4) Uani 1 1 d . . . C5 C 1.0210(3) 0.60997(14) 0.0633(2) 0.0209(5) Uani 1 1 d . . . H5 H 0.9326 0.6278 -0.0142 0.025 Uiso 1 1 calc R . . C6 C 1.1737(3) 0.63222(15) 0.0901(2) 0.0241(5) Uani 1 1 d . . . H6 H 1.1909 0.6669 0.0324 0.029 Uiso 1 1 calc R . . C7 C 1.3013(3) 0.60374(15) 0.2016(2) 0.0241(5) Uani 1 1 d . . . H7 H 1.4064 0.6182 0.2190 0.029 Uiso 1 1 calc R . . C8 C 1.2788(3) 0.55450(15) 0.2883(2) 0.0204(5) Uani 1 1 d . . . H8 H 1.3685 0.5358 0.3643 0.024 Uiso 1 1 calc R . . C9 C 0.8393(3) 0.53764(13) 0.1288(2) 0.0172(5) Uani 1 1 d . . . H9 H 0.7476 0.5520 0.0512 0.021 Uiso 1 1 calc R . . C10 C 0.6676(3) 0.47061(13) 0.1933(2) 0.0159(4) Uani 1 1 d . . . H10A H 0.5870 0.5103 0.1327 0.019 Uiso 1 1 calc R . . H10B H 0.6617 0.4720 0.2745 0.019 Uiso 1 1 calc R . . C11 C 0.6318(3) 0.38188(14) 0.1382(2) 0.0193(5) Uani 1 1 d . . . H11A H 0.6441 0.3799 0.0599 0.023 Uiso 1 1 calc R . . H11B H 0.7094 0.3420 0.2010 0.023 Uiso 1 1 calc R . . N2 N 0.4708(2) 0.35562(12) 0.10717(18) 0.0213(4) Uani 1 1 d . . . C12 C 0.4244(3) 0.28195(17) 0.0232(3) 0.0358(7) Uani 1 1 d . . . H12A H 0.4284 0.2960 -0.0557 0.054 Uiso 1 1 calc R . . H12B H 0.3159 0.2651 0.0024 0.054 Uiso 1 1 calc R . . H12C H 0.4978 0.2353 0.0666 0.054 Uiso 1 1 calc R . . C13 C 0.4593(3) 0.33619(18) 0.2228(2) 0.0325(6) Uani 1 1 d . . . H13A H 0.5372 0.2924 0.2717 0.049 Uiso 1 1 calc R . . H13B H 0.3518 0.3158 0.1993 0.049 Uiso 1 1 calc R . . H13C H 0.4812 0.3873 0.2752 0.049 Uiso 1 1 calc R . . C14 C 1.0609(3) 0.32547(14) 0.6079(2) 0.0228(5) Uani 1 1 d . . . H14A H 1.0756 0.2795 0.5592 0.034 Uiso 1 1 calc R . . H14B H 1.0108 0.3033 0.6575 0.034 Uiso 1 1 calc R . . H14C H 1.1646 0.3500 0.6662 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01091(5) 0.01035(4) 0.00976(4) -0.00016(3) 0.00303(3) 0.00155(3) S1 0.0155(3) 0.0110(2) 0.0135(3) -0.0004(2) 0.0061(2) -0.0001(2) N1 0.0122(9) 0.0113(8) 0.0127(9) -0.0018(7) 0.0027(8) -0.0009(7) C1 0.0203(12) 0.0138(10) 0.0187(12) -0.0037(9) 0.0077(10) 0.0022(9) C2 0.0133(11) 0.0193(10) 0.0152(11) 0.0006(9) 0.0029(9) 0.0025(9) C3 0.0187(11) 0.0145(10) 0.0130(10) -0.0009(8) 0.0076(9) 0.0002(9) C4 0.0163(11) 0.0154(10) 0.0157(11) 0.0000(8) 0.0083(9) 0.0005(9) C5 0.0246(13) 0.0223(12) 0.0143(11) 0.0038(9) 0.0078(10) 0.0019(10) C6 0.0305(14) 0.0257(12) 0.0227(13) 0.0016(10) 0.0180(12) -0.0039(10) C7 0.0202(12) 0.0310(13) 0.0258(13) -0.0001(11) 0.0147(11) -0.0039(10) C8 0.0147(12) 0.0261(12) 0.0170(12) 0.0004(9) 0.0047(10) 0.0008(9) C9 0.0182(11) 0.0154(10) 0.0125(11) 0.0008(8) 0.0027(9) 0.0029(9) C10 0.0123(11) 0.0171(10) 0.0155(11) -0.0008(8) 0.0042(9) 0.0001(8) C11 0.0146(11) 0.0192(11) 0.0212(12) -0.0029(9) 0.0062(10) -0.0025(9) N2 0.0175(10) 0.0196(10) 0.0232(11) -0.0045(8) 0.0066(9) -0.0057(8) C12 0.0292(15) 0.0278(13) 0.0423(17) -0.0105(12) 0.0101(13) -0.0122(12) C13 0.0285(15) 0.0354(15) 0.0360(16) -0.0002(12) 0.0171(13) -0.0096(12) C14 0.0306(14) 0.0135(10) 0.0236(13) 0.0039(9) 0.0122(11) 0.0065(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C3 2.020(2) . ? Pt1 C2 2.059(2) . ? Pt1 C1 2.076(2) . ? Pt1 N1 2.1538(19) . ? Pt1 S1 2.4352(7) . ? Pt1 S1 2.4439(8) 3_766 ? S1 C14 1.808(2) . ? S1 Pt1 2.4439(8) 3_766 ? N1 C9 1.279(3) . ? N1 C10 1.469(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C8 1.395(3) . ? C3 C4 1.409(3) . ? C4 C5 1.394(3) . ? C4 C9 1.449(3) . ? C5 C6 1.380(3) . ? C5 H5 0.9500 . ? C6 C7 1.382(3) . ? C6 H6 0.9500 . ? C7 C8 1.385(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.519(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N2 1.458(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N2 C13 1.459(3) . ? N2 C12 1.460(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Pt1 C2 91.54(9) . . ? C3 Pt1 C1 89.78(9) . . ? C2 Pt1 C1 87.35(9) . . ? C3 Pt1 N1 79.97(8) . . ? C2 Pt1 N1 170.75(8) . . ? C1 Pt1 N1 88.95(8) . . ? C3 Pt1 S1 171.34(6) . . ? C2 Pt1 S1 96.07(7) . . ? C1 Pt1 S1 94.70(7) . . ? N1 Pt1 S1 92.68(6) . . ? C3 Pt1 S1 93.37(6) . 3_766 ? C2 Pt1 S1 88.52(7) . 3_766 ? C1 Pt1 S1 174.88(6) . 3_766 ? N1 Pt1 S1 95.58(5) . 3_766 ? S1 Pt1 S1 82.72(3) . 3_766 ? C14 S1 Pt1 111.68(9) . . ? C14 S1 Pt1 108.61(8) . 3_766 ? Pt1 S1 Pt1 97.28(3) . 3_766 ? C9 N1 C10 118.19(19) . . ? C9 N1 Pt1 112.52(15) . . ? C10 N1 Pt1 129.08(14) . . ? Pt1 C1 H1A 109.5 . . ? Pt1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Pt1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Pt1 C2 H2A 109.5 . . ? Pt1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Pt1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C8 C3 C4 117.3(2) . . ? C8 C3 Pt1 129.80(17) . . ? C4 C3 Pt1 112.83(16) . . ? C5 C4 C3 121.6(2) . . ? C5 C4 C9 121.9(2) . . ? C3 C4 C9 116.5(2) . . ? C6 C5 C4 119.6(2) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 119.5(2) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C6 C7 C8 121.3(2) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C7 C8 C3 120.7(2) . . ? C7 C8 H8 119.6 . . ? C3 C8 H8 119.6 . . ? N1 C9 C4 118.1(2) . . ? N1 C9 H9 121.0 . . ? C4 C9 H9 121.0 . . ? N1 C10 C11 110.34(18) . . ? N1 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N1 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? N2 C11 C10 111.60(18) . . ? N2 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? N2 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 N2 C13 111.06(18) . . ? C11 N2 C12 110.10(19) . . ? C13 N2 C12 109.8(2) . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? S1 C14 H14A 109.5 . . ? S1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? S1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Pt1 S1 C14 -177.0(4) . . . . ? C2 Pt1 S1 C14 -25.67(10) . . . . ? C1 Pt1 S1 C14 62.16(11) . . . . ? N1 Pt1 S1 C14 151.32(10) . . . . ? S1 Pt1 S1 C14 -113.39(9) 3_766 . . . ? C3 Pt1 S1 Pt1 -63.6(4) . . . 3_766 ? C2 Pt1 S1 Pt1 87.72(7) . . . 3_766 ? C1 Pt1 S1 Pt1 175.55(6) . . . 3_766 ? N1 Pt1 S1 Pt1 -95.29(5) . . . 3_766 ? S1 Pt1 S1 Pt1 0.0 3_766 . . 3_766 ? C3 Pt1 N1 C9 0.74(15) . . . . ? C2 Pt1 N1 C9 -22.8(5) . . . . ? C1 Pt1 N1 C9 -89.22(16) . . . . ? S1 Pt1 N1 C9 176.12(15) . . . . ? S1 Pt1 N1 C9 93.18(15) 3_766 . . . ? C3 Pt1 N1 C10 175.32(18) . . . . ? C2 Pt1 N1 C10 151.8(4) . . . . ? C1 Pt1 N1 C10 85.36(18) . . . . ? S1 Pt1 N1 C10 -9.29(17) . . . . ? S1 Pt1 N1 C10 -92.23(17) 3_766 . . . ? C2 Pt1 C3 C8 -6.4(2) . . . . ? C1 Pt1 C3 C8 -93.8(2) . . . . ? N1 Pt1 C3 C8 177.2(2) . . . . ? S1 Pt1 C3 C8 145.0(3) . . . . ? S1 Pt1 C3 C8 82.2(2) 3_766 . . . ? C2 Pt1 C3 C4 177.68(16) . . . . ? C1 Pt1 C3 C4 90.33(16) . . . . ? N1 Pt1 C3 C4 1.36(15) . . . . ? S1 Pt1 C3 C4 -30.9(5) . . . . ? S1 Pt1 C3 C4 -93.72(15) 3_766 . . . ? C8 C3 C4 C5 0.3(3) . . . . ? Pt1 C3 C4 C5 176.77(17) . . . . ? C8 C3 C4 C9 -179.62(19) . . . . ? Pt1 C3 C4 C9 -3.2(2) . . . . ? C3 C4 C5 C6 -1.4(3) . . . . ? C9 C4 C5 C6 178.5(2) . . . . ? C4 C5 C6 C7 1.8(3) . . . . ? C5 C6 C7 C8 -1.2(4) . . . . ? C6 C7 C8 C3 0.1(4) . . . . ? C4 C3 C8 C7 0.3(3) . . . . ? Pt1 C3 C8 C7 -175.40(17) . . . . ? C10 N1 C9 C4 -177.94(18) . . . . ? Pt1 N1 C9 C4 -2.7(2) . . . . ? C5 C4 C9 N1 -175.9(2) . . . . ? C3 C4 C9 N1 4.1(3) . . . . ? C9 N1 C10 C11 92.6(2) . . . . ? Pt1 N1 C10 C11 -81.7(2) . . . . ? N1 C10 C11 N2 -176.90(18) . . . . ? C10 C11 N2 C13 -73.9(2) . . . . ? C10 C11 N2 C12 164.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.846 _diffrn_reflns_theta_full 28.91 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.881 _refine_diff_density_min -1.469 _refine_diff_density_rms 0.169 _database_code_depnum_ccdc_archive 'CCDC 933211' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_b13119 #TrackingRef '19315_web_deposit_cif_file_1_Puddephatt_1365538128.7b.cif' _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 N2 Pt2 S2' _chemical_formula_weight 904.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_H-M_alt 'C c' _space_group_name_Hall 'C -2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 20.627(6) _cell_length_b 9.269(3) _cell_length_c 16.440(4) _cell_angle_alpha 90 _cell_angle_beta 111.186(9) _cell_angle_gamma 90 _cell_volume 2930.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 110 _cell_measurement_reflns_used 9693 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 33.66 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.051 _exptl_crystal_F_000 1728 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.199 _exptl_crystal_size_mid 0.138 _exptl_crystal_size_min 0.052 _exptl_absorpt_coefficient_mu 9.704 _shelx_estimated_absorpt_T_min 0.248 _shelx_estimated_absorpt_T_max 0.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4945 _exptl_absorpt_correction_T_max 0.7472 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker Kappa Axis Apex2' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37458 _diffrn_reflns_av_unetI/netI 0.0466 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.314 _diffrn_reflns_theta_max 36.458 _diffrn_reflns_theta_full 33.430 _diffrn_measured_fraction_theta_max 0.874 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.874 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.643 _diffrn_reflns_point_group_measured_fraction_full 0.754 _reflns_number_total 9219 _reflns_number_gt 8661 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.469 _reflns_Friedel_fraction_max 0.411 _reflns_Friedel_fraction_full 0.512 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. These statistics refer to single and composite reflections containing twin component 1 only. ; _computing_data_collection Apex2 _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution XS _computing_structure_refinement SHELXL-2013 _computing_molecular_graphics NRCVAX _computing_publication_material cif2tables.py _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0166P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack -0.004(7) _chemical_absolute_configuration ? _refine_ls_number_reflns 9219 _refine_ls_number_parameters 350 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0464 _refine_ls_wR_factor_gt 0.0453 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.55674(2) 0.33406(2) 0.32226(2) 0.01095(4) Uani 1 1 d . . . . . Pt2 Pt 0.44291(2) 0.61167(2) 0.18328(2) 0.00958(3) Uani 1 1 d . . . . . S1 S 0.54881(6) 0.47823(12) 0.19490(8) 0.0118(2) Uani 1 1 d . . . . . S2 S 0.46561(6) 0.49969(12) 0.32697(8) 0.0119(2) Uani 1 1 d . . . . . C1 C 0.6359(3) 0.2028(6) 0.3150(4) 0.0219(11) Uani 1 1 d . . . . . H1A H 0.6800 0.2312 0.3602 0.033 Uiso 1 1 calc R U . . . H1B H 0.6394 0.2130 0.2574 0.033 Uiso 1 1 calc R U . . . H1C H 0.6256 0.1021 0.3241 0.033 Uiso 1 1 calc R U . . . C2 C 0.4867(3) 0.1904(5) 0.2444(4) 0.0202(10) Uani 1 1 d . . . . . H2A H 0.4616 0.1439 0.2777 0.030 Uiso 1 1 calc R U . . . H2B H 0.5112 0.1170 0.2236 0.030 Uiso 1 1 calc R U . . . H2C H 0.4536 0.2413 0.1943 0.030 Uiso 1 1 calc R U . . . C3 C 0.4308(3) 0.7148(6) 0.0671(3) 0.0164(9) Uani 1 1 d . . . . . H3A H 0.3833 0.6998 0.0256 0.025 Uiso 1 1 calc R U . . . H3B H 0.4640 0.6751 0.0428 0.025 Uiso 1 1 calc R U . . . H3C H 0.4393 0.8183 0.0777 0.025 Uiso 1 1 calc R U . . . C4 C 0.5121(2) 0.7714(5) 0.2478(3) 0.0158(9) Uani 1 1 d . . . . . H4A H 0.4997 0.8616 0.2146 0.024 Uiso 1 1 calc R U . . . H4B H 0.5593 0.7428 0.2535 0.024 Uiso 1 1 calc R U . . . H4C H 0.5101 0.7856 0.3059 0.024 Uiso 1 1 calc R U . . . C5 C 0.5670(2) 0.2257(5) 0.4330(3) 0.0149(9) Uani 1 1 d . . . . . C6 C 0.5390(3) 0.0944(5) 0.4445(4) 0.0215(11) Uani 1 1 d . . . . . H6 H 0.5085 0.0447 0.3949 0.026 Uiso 1 1 calc R U . . . C7 C 0.5542(3) 0.0340(6) 0.5265(4) 0.0281(12) Uani 1 1 d . . . . . H7 H 0.5349 -0.0568 0.5320 0.034 Uiso 1 1 calc R U . . . C8 C 0.5979(3) 0.1055(6) 0.6014(4) 0.0270(12) Uani 1 1 d . . . . . H8 H 0.6076 0.0647 0.6576 0.032 Uiso 1 1 calc R U . . . C9 C 0.6266(3) 0.2360(6) 0.5921(3) 0.0231(10) Uani 1 1 d . . . . . H9 H 0.6567 0.2856 0.6421 0.028 Uiso 1 1 calc R U . . . C10 C 0.6114(3) 0.2953(5) 0.5091(3) 0.0169(9) Uani 1 1 d . . . . . C11 C 0.6429(2) 0.4276(5) 0.4963(3) 0.0158(9) Uani 1 1 d . . . . . H11 H 0.6724 0.4810 0.5449 0.019 Uiso 1 1 calc R U . . . N1 N 0.6305(2) 0.4725(4) 0.4184(3) 0.0129(7) Uani 1 1 d . . . . . C12 C 0.6608(3) 0.6052(5) 0.4061(3) 0.0143(8) Uani 1 1 d . . . . . C13 C 0.6488(3) 0.7323(6) 0.4423(3) 0.0176(9) Uani 1 1 d . . . . . H13 H 0.6204 0.7322 0.4767 0.021 Uiso 1 1 calc R U . . . C14 C 0.6781(3) 0.8597(5) 0.4283(3) 0.0181(10) Uani 1 1 d . . . . . H14 H 0.6691 0.9470 0.4525 0.022 Uiso 1 1 calc R U . . . C15 C 0.7205(3) 0.8614(5) 0.3797(4) 0.0202(10) Uani 1 1 d . . . . . H15 H 0.7412 0.9490 0.3714 0.024 Uiso 1 1 calc R U . . . C16 C 0.7323(2) 0.7346(5) 0.3430(3) 0.0194(9) Uani 1 1 d . . . . . H16 H 0.7614 0.7352 0.3096 0.023 Uiso 1 1 calc R U . . . C17 C 0.7018(3) 0.6054(5) 0.3547(3) 0.0164(9) Uani 1 1 d . . . . . H17 H 0.7089 0.5189 0.3280 0.020 Uiso 1 1 calc R U . . . C18 C 0.3624(2) 0.7272(5) 0.1899(3) 0.0127(8) Uani 1 1 d . . . . . C19 C 0.3627(3) 0.8660(5) 0.2217(3) 0.0152(9) Uani 1 1 d . . . . . H19 H 0.4047 0.9197 0.2415 0.018 Uiso 1 1 calc R U . . . C20 C 0.3020(3) 0.9273(5) 0.2248(3) 0.0175(9) Uani 1 1 d . . . . . H20 H 0.3034 1.0227 0.2466 0.021 Uiso 1 1 calc R U . . . C21 C 0.2398(3) 0.8528(5) 0.1970(3) 0.0187(9) Uani 1 1 d . . . . . H21 H 0.1991 0.8957 0.2006 0.022 Uiso 1 1 calc R U . . . C22 C 0.2375(3) 0.7140(6) 0.1636(3) 0.0191(9) Uani 1 1 d . . . . . H22 H 0.1952 0.6610 0.1439 0.023 Uiso 1 1 calc R U . . . C23 C 0.2984(3) 0.6539(5) 0.1596(3) 0.0149(8) Uani 1 1 d . . . . . C24 C 0.2973(2) 0.5164(5) 0.1168(3) 0.0145(8) Uani 1 1 d . . . . . H24 H 0.2555 0.4624 0.0936 0.017 Uiso 1 1 calc R U . . . N2 N 0.3542(2) 0.4693(4) 0.1111(2) 0.0132(7) Uani 1 1 d . . . . . C25 C 0.3504(3) 0.3435(5) 0.0597(3) 0.0145(9) Uani 1 1 d . . . . . C26 C 0.3765(3) 0.3524(5) -0.0074(3) 0.0162(9) Uani 1 1 d . . . . . H26 H 0.3950 0.4409 -0.0187 0.019 Uiso 1 1 calc R U . . . C27 C 0.3753(3) 0.2312(6) -0.0579(3) 0.0224(10) Uani 1 1 d . . . . . H27 H 0.3920 0.2375 -0.1046 0.027 Uiso 1 1 calc R U . . . C28 C 0.3499(3) 0.1016(5) -0.0402(4) 0.0229(11) Uani 1 1 d . . . . . H28 H 0.3501 0.0184 -0.0739 0.027 Uiso 1 1 calc R U . . . C29 C 0.3242(3) 0.0934(5) 0.0264(3) 0.0185(10) Uani 1 1 d . . . . . H29 H 0.3066 0.0045 0.0385 0.022 Uiso 1 1 calc R U . . . C30 C 0.3241(3) 0.2144(5) 0.0756(3) 0.0181(9) Uani 1 1 d . . . . . H30 H 0.3058 0.2085 0.1208 0.022 Uiso 1 1 calc R U . . . C31 C 0.5401(3) 0.3592(6) 0.1043(3) 0.0208(10) Uani 1 1 d . . . . . H31A H 0.5842 0.3086 0.1151 0.031 Uiso 1 1 calc R U . . . H31B H 0.5282 0.4158 0.0506 0.031 Uiso 1 1 calc R U . . . H31C H 0.5033 0.2886 0.0983 0.031 Uiso 1 1 calc R U . . . C32 C 0.3907(3) 0.3927(5) 0.3217(3) 0.0187(9) Uani 1 1 d . . . . . H32A H 0.3780 0.3284 0.2710 0.028 Uiso 1 1 calc R U . . . H32B H 0.3515 0.4568 0.3163 0.028 Uiso 1 1 calc R U . . . H32C H 0.4019 0.3350 0.3750 0.028 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01307(8) 0.00702(7) 0.01401(7) 0.00056(6) 0.00640(6) 0.00050(7) Pt2 0.01096(7) 0.00771(7) 0.01055(7) -0.00052(6) 0.00447(5) -0.00063(6) S1 0.0125(5) 0.0111(5) 0.0128(5) -0.0007(4) 0.0059(4) 0.0003(4) S2 0.0135(5) 0.0111(4) 0.0121(5) -0.0002(4) 0.0058(4) 0.0003(4) C1 0.025(3) 0.018(2) 0.027(3) 0.004(2) 0.014(2) 0.008(2) C2 0.025(3) 0.010(2) 0.029(3) -0.0016(18) 0.014(2) -0.0026(18) C3 0.021(2) 0.016(2) 0.015(2) 0.0023(17) 0.0087(18) -0.0001(19) C4 0.013(2) 0.0117(19) 0.020(2) -0.0055(17) 0.0032(18) -0.0025(17) C5 0.017(2) 0.0125(19) 0.020(2) 0.0062(17) 0.0127(18) 0.0055(17) C6 0.025(3) 0.012(2) 0.033(3) 0.0048(19) 0.017(2) 0.0032(18) C7 0.037(3) 0.018(2) 0.040(3) 0.010(2) 0.027(3) 0.006(2) C8 0.032(3) 0.030(3) 0.029(3) 0.018(2) 0.023(2) 0.015(2) C9 0.029(3) 0.025(3) 0.018(2) 0.0074(19) 0.012(2) 0.009(2) C10 0.019(2) 0.018(2) 0.018(2) 0.0055(17) 0.0117(19) 0.0060(18) C11 0.010(2) 0.021(2) 0.015(2) 0.0007(17) 0.0030(16) 0.0025(17) N1 0.0105(17) 0.0133(17) 0.0142(18) 0.0002(13) 0.0036(14) 0.0015(13) C12 0.015(2) 0.014(2) 0.013(2) -0.0002(16) 0.0042(17) 0.0006(16) C13 0.017(2) 0.022(2) 0.013(2) 0.0021(18) 0.0047(18) 0.0052(19) C14 0.020(2) 0.010(2) 0.022(2) -0.0026(17) 0.006(2) 0.0009(17) C15 0.019(2) 0.013(2) 0.026(3) 0.0006(18) 0.005(2) -0.0060(18) C16 0.015(2) 0.020(2) 0.024(3) 0.0002(19) 0.0088(19) 0.0008(18) C17 0.016(2) 0.0122(19) 0.021(2) -0.0022(17) 0.0065(18) -0.0013(16) C18 0.015(2) 0.0128(19) 0.013(2) 0.0030(16) 0.0077(17) 0.0019(16) C19 0.020(2) 0.0099(18) 0.017(2) 0.0006(16) 0.0083(19) 0.0014(16) C20 0.024(2) 0.013(2) 0.018(2) 0.0007(17) 0.0105(19) 0.0058(18) C21 0.021(2) 0.021(2) 0.016(2) 0.0010(18) 0.0087(19) 0.0069(19) C22 0.016(2) 0.023(2) 0.018(2) -0.0016(18) 0.0060(18) 0.0019(19) C23 0.016(2) 0.016(2) 0.015(2) 0.0002(16) 0.0065(17) 0.0011(16) C24 0.014(2) 0.0131(19) 0.013(2) 0.0013(16) 0.0008(16) -0.0024(16) N2 0.017(2) 0.0128(17) 0.0093(17) -0.0030(13) 0.0043(15) -0.0024(14) C25 0.013(2) 0.016(2) 0.014(2) -0.0015(17) 0.0030(17) -0.0005(17) C26 0.021(2) 0.015(2) 0.015(2) -0.0023(16) 0.0082(18) -0.0053(17) C27 0.025(3) 0.025(2) 0.020(2) -0.007(2) 0.011(2) -0.006(2) C28 0.028(3) 0.017(2) 0.024(3) -0.0074(19) 0.009(2) -0.002(2) C29 0.022(2) 0.015(2) 0.016(2) -0.0023(16) 0.0047(19) -0.0067(18) C30 0.021(3) 0.018(2) 0.015(2) -0.0021(18) 0.0052(19) -0.005(2) C31 0.019(2) 0.025(2) 0.018(2) -0.0065(19) 0.0069(19) 0.0049(19) C32 0.018(2) 0.024(2) 0.016(2) 0.0026(18) 0.0084(18) -0.0028(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C5 2.022(5) . ? Pt1 C2 2.041(5) . ? Pt1 C1 2.074(5) . ? Pt1 N1 2.173(4) . ? Pt1 S1 2.4391(13) . ? Pt1 S2 2.4497(13) . ? Pt2 C18 2.012(5) . ? Pt2 C4 2.064(5) . ? Pt2 C3 2.069(5) . ? Pt2 N2 2.220(4) . ? Pt2 S1 2.4569(13) . ? Pt2 S2 2.4652(13) . ? S1 C31 1.809(5) . ? S2 C32 1.813(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.390(7) . ? C5 C10 1.411(7) . ? C6 C7 1.386(8) . ? C6 H6 0.9500 . ? C7 C8 1.402(9) . ? C7 H7 0.9500 . ? C8 C9 1.379(8) . ? C8 H8 0.9500 . ? C9 C10 1.397(7) . ? C9 H9 0.9500 . ? C10 C11 1.438(7) . ? C11 N1 1.280(6) . ? C11 H11 0.9500 . ? N1 C12 1.428(6) . ? C12 C13 1.381(7) . ? C12 C17 1.396(7) . ? C13 C14 1.383(7) . ? C13 H13 0.9500 . ? C14 C15 1.381(8) . ? C14 H14 0.9500 . ? C15 C16 1.383(7) . ? C15 H15 0.9500 . ? C16 C17 1.397(7) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.388(6) . ? C18 C23 1.406(7) . ? C19 C20 1.392(7) . ? C19 H19 0.9500 . ? C20 C21 1.382(7) . ? C20 H20 0.9500 . ? C21 C22 1.393(7) . ? C21 H21 0.9500 . ? C22 C23 1.398(7) . ? C22 H22 0.9500 . ? C23 C24 1.451(7) . ? C24 N2 1.287(6) . ? C24 H24 0.9500 . ? N2 C25 1.426(6) . ? C25 C30 1.377(7) . ? C25 C26 1.393(7) . ? C26 C27 1.392(7) . ? C26 H26 0.9500 . ? C27 C28 1.382(7) . ? C27 H27 0.9500 . ? C28 C29 1.381(8) . ? C28 H28 0.9500 . ? C29 C30 1.384(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pt1 C2 93.5(2) . . ? C5 Pt1 C1 86.1(2) . . ? C2 Pt1 C1 88.6(2) . . ? C5 Pt1 N1 79.64(18) . . ? C2 Pt1 N1 173.09(19) . . ? C1 Pt1 N1 91.69(19) . . ? C5 Pt1 S1 176.09(15) . . ? C2 Pt1 S1 90.35(15) . . ? C1 Pt1 S1 94.72(16) . . ? N1 Pt1 S1 96.51(11) . . ? C5 Pt1 S2 96.60(13) . . ? C2 Pt1 S2 92.94(15) . . ? C1 Pt1 S2 176.86(16) . . ? N1 Pt1 S2 87.16(11) . . ? S1 Pt1 S2 82.51(4) . . ? C18 Pt2 C4 91.2(2) . . ? C18 Pt2 C3 88.72(19) . . ? C4 Pt2 C3 88.5(2) . . ? C18 Pt2 N2 78.94(17) . . ? C4 Pt2 N2 169.86(17) . . ? C3 Pt2 N2 88.83(18) . . ? C18 Pt2 S1 172.69(14) . . ? C4 Pt2 S1 83.75(14) . . ? C3 Pt2 S1 96.42(14) . . ? N2 Pt2 S1 106.28(11) . . ? C18 Pt2 S2 92.66(13) . . ? C4 Pt2 S2 87.30(15) . . ? C3 Pt2 S2 175.59(15) . . ? N2 Pt2 S2 95.54(10) . . ? S1 Pt2 S2 81.83(4) . . ? C31 S1 Pt1 109.16(19) . . ? C31 S1 Pt2 114.97(17) . . ? Pt1 S1 Pt2 97.15(4) . . ? C32 S2 Pt1 107.86(17) . . ? C32 S2 Pt2 108.75(17) . . ? Pt1 S2 Pt2 96.65(4) . . ? Pt1 C1 H1A 109.5 . . ? Pt1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Pt1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Pt1 C2 H2A 109.5 . . ? Pt1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Pt1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Pt2 C3 H3A 109.5 . . ? Pt2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Pt2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Pt2 C4 H4A 109.5 . . ? Pt2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Pt2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C10 116.6(4) . . ? C6 C5 Pt1 130.1(4) . . ? C10 C5 Pt1 113.2(3) . . ? C7 C6 C5 121.8(5) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C8 120.8(5) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C7 118.8(5) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C10 120.0(5) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C5 122.0(5) . . ? C9 C10 C11 121.7(5) . . ? C5 C10 C11 116.3(4) . . ? N1 C11 C10 119.1(4) . . ? N1 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 N1 C12 118.8(4) . . ? C11 N1 Pt1 111.7(3) . . ? C12 N1 Pt1 129.3(3) . . ? C13 C12 C17 120.1(5) . . ? C13 C12 N1 121.2(5) . . ? C17 C12 N1 118.6(4) . . ? C12 C13 C14 119.9(5) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.8(5) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.4(5) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 120.6(5) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C12 C17 C16 119.0(4) . . ? C12 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C19 C18 C23 117.2(4) . . ? C19 C18 Pt2 128.5(4) . . ? C23 C18 Pt2 114.3(3) . . ? C18 C19 C20 120.8(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 121.5(4) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 119.2(5) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C21 C22 C23 118.9(5) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C22 C23 C18 122.4(4) . . ? C22 C23 C24 121.1(4) . . ? C18 C23 C24 116.4(4) . . ? N2 C24 C23 118.6(4) . . ? N2 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C24 N2 C25 117.7(4) . . ? C24 N2 Pt2 110.9(3) . . ? C25 N2 Pt2 131.4(3) . . ? C30 C25 C26 119.5(5) . . ? C30 C25 N2 122.6(5) . . ? C26 C25 N2 117.8(4) . . ? C27 C26 C25 119.7(5) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 120.2(5) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C29 C28 C27 119.8(5) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 120.1(5) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C25 C30 C29 120.6(5) . . ? C25 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? S1 C31 H31A 109.5 . . ? S1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S2 C32 H32A 109.5 . . ? S2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C5 C6 C7 -0.6(7) . . . . ? Pt1 C5 C6 C7 177.5(4) . . . . ? C5 C6 C7 C8 1.2(8) . . . . ? C6 C7 C8 C9 -1.2(8) . . . . ? C7 C8 C9 C10 0.5(8) . . . . ? C8 C9 C10 C5 0.1(8) . . . . ? C8 C9 C10 C11 -176.9(5) . . . . ? C6 C5 C10 C9 -0.1(7) . . . . ? Pt1 C5 C10 C9 -178.4(4) . . . . ? C6 C5 C10 C11 177.1(4) . . . . ? Pt1 C5 C10 C11 -1.3(5) . . . . ? C9 C10 C11 N1 175.7(4) . . . . ? C5 C10 C11 N1 -1.5(7) . . . . ? C10 C11 N1 C12 178.9(4) . . . . ? C10 C11 N1 Pt1 3.3(5) . . . . ? C11 N1 C12 C13 -57.7(6) . . . . ? Pt1 N1 C12 C13 117.0(5) . . . . ? C11 N1 C12 C17 123.9(5) . . . . ? Pt1 N1 C12 C17 -61.3(6) . . . . ? C17 C12 C13 C14 -0.8(7) . . . . ? N1 C12 C13 C14 -179.2(4) . . . . ? C12 C13 C14 C15 -1.0(8) . . . . ? C13 C14 C15 C16 1.4(8) . . . . ? C14 C15 C16 C17 0.1(8) . . . . ? C13 C12 C17 C16 2.2(7) . . . . ? N1 C12 C17 C16 -179.4(4) . . . . ? C15 C16 C17 C12 -1.9(8) . . . . ? C23 C18 C19 C20 1.5(7) . . . . ? Pt2 C18 C19 C20 -177.1(4) . . . . ? C18 C19 C20 C21 0.3(7) . . . . ? C19 C20 C21 C22 -1.2(7) . . . . ? C20 C21 C22 C23 0.3(7) . . . . ? C21 C22 C23 C18 1.6(7) . . . . ? C21 C22 C23 C24 -173.2(4) . . . . ? C19 C18 C23 C22 -2.4(7) . . . . ? Pt2 C18 C23 C22 176.4(4) . . . . ? C19 C18 C23 C24 172.6(4) . . . . ? Pt2 C18 C23 C24 -8.6(5) . . . . ? C22 C23 C24 N2 176.6(4) . . . . ? C18 C23 C24 N2 1.5(6) . . . . ? C23 C24 N2 C25 -172.4(4) . . . . ? C23 C24 N2 Pt2 5.6(5) . . . . ? C24 N2 C25 C30 -57.4(6) . . . . ? Pt2 N2 C25 C30 125.1(5) . . . . ? C24 N2 C25 C26 124.5(5) . . . . ? Pt2 N2 C25 C26 -53.0(6) . . . . ? C30 C25 C26 C27 0.4(8) . . . . ? N2 C25 C26 C27 178.5(5) . . . . ? C25 C26 C27 C28 -1.5(8) . . . . ? C26 C27 C28 C29 1.4(8) . . . . ? C27 C28 C29 C30 -0.2(8) . . . . ? C26 C25 C30 C29 0.9(8) . . . . ? N2 C25 C30 C29 -177.2(5) . . . . ? C28 C29 C30 C25 -1.0(8) . . . . ? _refine_diff_density_max 2.800 _refine_diff_density_min -2.080 _refine_diff_density_rms 0.189 _database_code_depnum_ccdc_archive 'CCDC 933212' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_7a _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 N2 Pt2 S2' _chemical_formula_weight 904.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.461(5) _cell_length_b 9.198(6) _cell_length_c 11.156(5) _cell_angle_alpha 93.302(8) _cell_angle_beta 109.27(3) _cell_angle_gamma 108.338(14) _cell_volume 765.2(8) _cell_formula_units_Z 1 _cell_measurement_temperature 150 _cell_measurement_reflns_used 9893 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 33.40 _exptl_crystal_description prism _exptl_crystal_colour 'pale greenish yellow' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.964 _exptl_crystal_F_000 432 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.466 _exptl_crystal_size_mid 0.254 _exptl_crystal_size_min 0.091 _exptl_absorpt_coefficient_mu 9.291 _shelx_estimated_absorpt_T_min 0.098 _shelx_estimated_absorpt_T_max 0.485 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4615 _exptl_absorpt_correction_T_max 0.7468 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21667 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.824 _diffrn_reflns_theta_max 34.985 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.936 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.936 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.936 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 6292 _reflns_number_gt 5508 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection Apex2 _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution SIR92 _computing_structure_refinement SHELXL-2013 _computing_molecular_graphics NRCVAX _computing_publication_material cif2tables.py _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+0.6604P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6292 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0507 _refine_ls_wR_factor_gt 0.0488 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.35141(2) 0.08496(2) 0.39376(2) 0.01362(3) Uani 1 1 d . . . . . S1 S 0.63638(9) 0.05061(8) 0.42342(7) 0.01664(13) Uani 1 1 d . . . . . C1 C 0.1232(4) 0.1294(4) 0.3854(3) 0.0237(6) Uani 1 1 d . . . . . H1A H 0.1477 0.2416 0.3925 0.036 Uiso 1 1 calc R U . . . H1B H 0.0878 0.0927 0.4567 0.036 Uiso 1 1 calc R U . . . H1C H 0.0261 0.0749 0.3030 0.036 Uiso 1 1 calc R U . . . C2 C 0.5015(4) 0.2972(3) 0.5128(3) 0.0251(6) Uani 1 1 d . . . . . H2A H 0.6020 0.3499 0.4869 0.038 Uiso 1 1 calc R U . . . H2B H 0.5475 0.2818 0.6022 0.038 Uiso 1 1 calc R U . . . H2C H 0.4266 0.3611 0.5062 0.038 Uiso 1 1 calc R U . . . C3 C 0.3408(4) 0.1770(3) 0.2325(3) 0.0191(5) Uani 1 1 d . . . . . C4 C 0.4050(4) 0.3329(4) 0.2188(3) 0.0263(6) Uani 1 1 d . . . . . H4 H 0.4614 0.4127 0.2931 0.032 Uiso 1 1 calc R U . . . C5 C 0.3870(5) 0.3725(4) 0.0974(3) 0.0319(7) Uani 1 1 d . . . . . H5 H 0.4302 0.4791 0.0904 0.038 Uiso 1 1 calc R U . . . C6 C 0.3070(5) 0.2588(4) -0.0136(3) 0.0335(8) Uani 1 1 d . . . . . H6 H 0.2983 0.2875 -0.0954 0.040 Uiso 1 1 calc R U . . . C7 C 0.2406(5) 0.1047(4) -0.0040(3) 0.0310(7) Uani 1 1 d . . . . . H7 H 0.1850 0.0262 -0.0792 0.037 Uiso 1 1 calc R U . . . C8 C 0.2555(4) 0.0639(4) 0.1175(3) 0.0224(6) Uani 1 1 d . . . . . C9 C 0.1732(4) -0.0943(4) 0.1315(3) 0.0230(6) Uani 1 1 d . . . . . H9 H 0.1104 -0.1751 0.0578 0.028 Uiso 1 1 calc R U . . . N1 N 0.1861(3) -0.1246(3) 0.2450(2) 0.0172(4) Uani 1 1 d . . . . . C10 C 0.0935(4) -0.2791(3) 0.2569(3) 0.0194(5) Uani 1 1 d . . . . . C11 C -0.0028(4) -0.2988(3) 0.3383(3) 0.0214(6) Uani 1 1 d . . . . . H11 H -0.0024 -0.2103 0.3869 0.026 Uiso 1 1 calc R U . . . C12 C -0.0996(4) -0.4478(4) 0.3489(3) 0.0285(7) Uani 1 1 d . . . . . H12 H -0.1668 -0.4607 0.4035 0.034 Uiso 1 1 calc R U . . . C13 C -0.0981(5) -0.5778(4) 0.2799(4) 0.0360(8) Uani 1 1 d . . . . . H13 H -0.1652 -0.6795 0.2863 0.043 Uiso 1 1 calc R U . . . C14 C 0.0022(5) -0.5577(4) 0.2015(4) 0.0364(8) Uani 1 1 d . . . . . H14 H 0.0061 -0.6464 0.1562 0.044 Uiso 1 1 calc R U . . . C15 C 0.0970(5) -0.4098(4) 0.1881(3) 0.0278(7) Uani 1 1 d . . . . . H15 H 0.1635 -0.3973 0.1330 0.033 Uiso 1 1 calc R U . . . C16 C 0.6121(4) -0.0757(4) 0.2820(3) 0.0274(7) Uani 1 1 d . . . . . H16A H 0.5020 -0.1668 0.2582 0.041 Uiso 1 1 calc R U . . . H16B H 0.7152 -0.1096 0.3016 0.041 Uiso 1 1 calc R U . . . H16C H 0.6059 -0.0186 0.2101 0.041 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01459(5) 0.01415(5) 0.01171(5) 0.00145(3) 0.00458(3) 0.00495(3) S1 0.0154(3) 0.0203(3) 0.0142(3) 0.0034(2) 0.0061(2) 0.0056(2) C1 0.0250(15) 0.0278(15) 0.0234(15) 0.0060(12) 0.0107(12) 0.0141(12) C2 0.0324(17) 0.0173(13) 0.0207(15) -0.0002(11) 0.0060(13) 0.0069(12) C3 0.0164(12) 0.0233(13) 0.0185(13) 0.0062(11) 0.0073(10) 0.0069(10) C4 0.0310(17) 0.0257(15) 0.0245(16) 0.0095(12) 0.0132(13) 0.0090(13) C5 0.0332(18) 0.0350(18) 0.0321(18) 0.0197(15) 0.0174(15) 0.0099(14) C6 0.0289(17) 0.050(2) 0.0237(16) 0.0190(15) 0.0118(14) 0.0115(15) C7 0.0275(16) 0.045(2) 0.0144(14) 0.0076(13) 0.0059(12) 0.0069(15) C8 0.0204(14) 0.0293(15) 0.0152(13) 0.0051(11) 0.0054(11) 0.0068(12) C9 0.0221(14) 0.0274(15) 0.0147(13) -0.0014(11) 0.0044(11) 0.0057(12) N1 0.0159(11) 0.0210(11) 0.0132(10) 0.0021(9) 0.0045(9) 0.0058(9) C10 0.0173(13) 0.0201(13) 0.0168(13) 0.0011(10) 0.0035(10) 0.0048(10) C11 0.0192(13) 0.0240(14) 0.0173(13) 0.0023(11) 0.0041(11) 0.0060(11) C12 0.0219(15) 0.0291(16) 0.0302(17) 0.0082(13) 0.0087(13) 0.0036(12) C13 0.0346(19) 0.0207(15) 0.039(2) 0.0086(14) 0.0048(16) 0.0007(14) C14 0.046(2) 0.0210(15) 0.0322(19) -0.0026(13) 0.0061(16) 0.0091(15) C15 0.0304(17) 0.0262(15) 0.0232(15) -0.0020(12) 0.0079(13) 0.0085(13) C16 0.0264(15) 0.0399(18) 0.0198(15) 0.0015(13) 0.0113(12) 0.0147(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C3 2.020(3) . ? Pt1 C2 2.053(3) . ? Pt1 C1 2.070(3) . ? Pt1 N1 2.197(3) . ? Pt1 S1 2.4414(12) 2_656 ? Pt1 S1 2.4470(15) . ? S1 C16 1.818(3) . ? S1 Pt1 2.4414(12) 2_656 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.401(4) . ? C3 C8 1.418(4) . ? C4 C5 1.394(5) . ? C4 H4 0.9500 . ? C5 C6 1.392(5) . ? C5 H5 0.9500 . ? C6 C7 1.376(5) . ? C6 H6 0.9500 . ? C7 C8 1.403(4) . ? C7 H7 0.9500 . ? C8 C9 1.445(4) . ? C9 N1 1.290(4) . ? C9 H9 0.9500 . ? N1 C10 1.429(4) . ? C10 C11 1.391(4) . ? C10 C15 1.402(4) . ? C11 C12 1.393(4) . ? C11 H11 0.9500 . ? C12 C13 1.390(5) . ? C12 H12 0.9500 . ? C13 C14 1.390(6) . ? C13 H13 0.9500 . ? C14 C15 1.390(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Pt1 C2 92.81(13) . . ? C3 Pt1 C1 88.49(12) . . ? C2 Pt1 C1 88.53(14) . . ? C3 Pt1 N1 79.64(11) . . ? C2 Pt1 N1 172.33(11) . . ? C1 Pt1 N1 89.94(12) . . ? C3 Pt1 S1 174.08(8) . 2_656 ? C2 Pt1 S1 92.20(10) . 2_656 ? C1 Pt1 S1 94.79(9) . 2_656 ? N1 Pt1 S1 95.41(8) . 2_656 ? C3 Pt1 S1 93.91(9) . . ? C2 Pt1 S1 86.33(10) . . ? C1 Pt1 S1 174.43(9) . . ? N1 Pt1 S1 95.44(7) . . ? S1 Pt1 S1 83.27(3) 2_656 . ? C16 S1 Pt1 111.38(12) . 2_656 ? C16 S1 Pt1 109.45(11) . . ? Pt1 S1 Pt1 96.73(3) 2_656 . ? Pt1 C1 H1A 109.5 . . ? Pt1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Pt1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Pt1 C2 H2A 109.5 . . ? Pt1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Pt1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C8 116.7(3) . . ? C4 C3 Pt1 129.8(2) . . ? C8 C3 Pt1 113.5(2) . . ? C5 C4 C3 120.9(3) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 121.2(3) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C7 C6 C5 119.4(3) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 119.7(3) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C3 122.0(3) . . ? C7 C8 C9 121.7(3) . . ? C3 C8 C9 116.1(3) . . ? N1 C9 C8 119.2(3) . . ? N1 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 N1 C10 118.8(2) . . ? C9 N1 Pt1 111.0(2) . . ? C10 N1 Pt1 130.18(19) . . ? C11 C10 C15 119.8(3) . . ? C11 C10 N1 118.7(3) . . ? C15 C10 N1 121.5(3) . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 119.4(3) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 121.0(3) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C10 119.2(3) . . ? C14 C15 H15 120.4 . . ? C10 C15 H15 120.4 . . ? S1 C16 H16A 109.5 . . ? S1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 C3 C4 C5 -0.9(5) . . . . ? Pt1 C3 C4 C5 178.8(2) . . . . ? C3 C4 C5 C6 -0.8(5) . . . . ? C4 C5 C6 C7 1.5(5) . . . . ? C5 C6 C7 C8 -0.5(5) . . . . ? C6 C7 C8 C3 -1.3(5) . . . . ? C6 C7 C8 C9 174.0(3) . . . . ? C4 C3 C8 C7 2.0(5) . . . . ? Pt1 C3 C8 C7 -177.8(3) . . . . ? C4 C3 C8 C9 -173.6(3) . . . . ? Pt1 C3 C8 C9 6.6(4) . . . . ? C7 C8 C9 N1 -177.7(3) . . . . ? C3 C8 C9 N1 -2.1(4) . . . . ? C8 C9 N1 C10 175.5(3) . . . . ? C8 C9 N1 Pt1 -3.1(3) . . . . ? C9 N1 C10 C11 -134.6(3) . . . . ? Pt1 N1 C10 C11 43.7(4) . . . . ? C9 N1 C10 C15 45.0(4) . . . . ? Pt1 N1 C10 C15 -136.7(3) . . . . ? C15 C10 C11 C12 -1.8(4) . . . . ? N1 C10 C11 C12 177.8(3) . . . . ? C10 C11 C12 C13 1.1(5) . . . . ? C11 C12 C13 C14 0.7(5) . . . . ? C12 C13 C14 C15 -1.8(6) . . . . ? C13 C14 C15 C10 1.1(5) . . . . ? C11 C10 C15 C14 0.7(5) . . . . ? N1 C10 C15 C14 -178.9(3) . . . . ? _refine_diff_density_max 1.276 _refine_diff_density_min -1.363 _refine_diff_density_rms 0.200 _shelxl_version_number 2012-9 _shelx_res_file ; TITL n13065: P-1 CELL 0.71073 8.46089 9.19790 11.15616 93.3023 109.2749 108.3384 ZERR 1 0.00483 0.00571 0.00534 0.0075 0.0259 0.0136 LATT 1 SFAC C H N PT S UNIT 32 38 2 2 2 TEMP -123 SIZE 0.466 0.254 0.091 ACTA MERG 2 REM omit reflections blocked by beam stop OMIT 1 0 0 OMIT 0 1 0 OMIT 0 0 1 OMIT 0 -1 1 OMIT -1 1 1 L.S. 12 FMAP 2 PLAN 30 BOND $H CONF HTAB WGHT 0.014700 0.660400 FVAR 0.15300 MOLE 1 PT1 4 0.351405 0.084957 0.393761 11.00000 0.01459 0.01415 = 0.01171 0.00145 0.00458 0.00495 S1 5 0.636384 0.050609 0.423419 11.00000 0.01543 0.02034 = 0.01417 0.00340 0.00613 0.00558 C1 1 0.123211 0.129386 0.385391 11.00000 0.02504 0.02785 = 0.02339 0.00602 0.01068 0.01405 AFIX 137 H1A 2 0.147682 0.241641 0.392543 11.00000 -1.50000 H1B 2 0.087824 0.092675 0.456665 11.00000 -1.50000 H1C 2 0.026097 0.074873 0.303004 11.00000 -1.50000 AFIX 0 C2 1 0.501497 0.297167 0.512833 11.00000 0.03239 0.01727 = 0.02072 -0.00023 0.00603 0.00693 AFIX 137 H2A 2 0.601986 0.349916 0.486943 11.00000 -1.50000 H2B 2 0.547514 0.281811 0.602216 11.00000 -1.50000 H2C 2 0.426638 0.361070 0.506178 11.00000 -1.50000 AFIX 0 C3 1 0.340819 0.177044 0.232477 11.00000 0.01636 0.02334 = 0.01846 0.00622 0.00731 0.00686 C4 1 0.404962 0.332898 0.218756 11.00000 0.03099 0.02572 = 0.02455 0.00945 0.01316 0.00898 AFIX 43 H4 2 0.461440 0.412651 0.293134 11.00000 -1.20000 AFIX 0 C5 1 0.387022 0.372504 0.097447 11.00000 0.03323 0.03503 = 0.03206 0.01970 0.01743 0.00989 AFIX 43 H5 2 0.430213 0.479056 0.090436 11.00000 -1.20000 AFIX 0 C6 1 0.307003 0.258849 -0.013616 11.00000 0.02888 0.04959 = 0.02366 0.01901 0.01181 0.01150 AFIX 43 H6 2 0.298285 0.287467 -0.095393 11.00000 -1.20000 AFIX 0 C7 1 0.240631 0.104688 -0.003960 11.00000 0.02749 0.04533 = 0.01439 0.00763 0.00590 0.00688 AFIX 43 H7 2 0.184972 0.026233 -0.079200 11.00000 -1.20000 AFIX 0 C8 1 0.255546 0.063930 0.117508 11.00000 0.02037 0.02926 = 0.01522 0.00508 0.00541 0.00681 C9 1 0.173245 -0.094310 0.131454 11.00000 0.02210 0.02738 = 0.01469 -0.00138 0.00442 0.00575 AFIX 43 H9 2 0.110398 -0.175114 0.057823 11.00000 -1.20000 AFIX 0 N1 3 0.186081 -0.124603 0.245016 11.00000 0.01590 0.02096 = 0.01321 0.00208 0.00449 0.00576 C10 1 0.093473 -0.279124 0.256911 11.00000 0.01731 0.02010 = 0.01679 0.00106 0.00348 0.00480 C11 1 -0.002750 -0.298822 0.338326 11.00000 0.01921 0.02396 = 0.01733 0.00228 0.00412 0.00595 AFIX 43 H11 2 -0.002413 -0.210325 0.386861 11.00000 -1.20000 AFIX 0 C12 1 -0.099597 -0.447840 0.348942 11.00000 0.02194 0.02907 = 0.03016 0.00824 0.00873 0.00357 AFIX 43 H12 2 -0.166810 -0.460679 0.403508 11.00000 -1.20000 AFIX 0 C13 1 -0.098140 -0.577779 0.279908 11.00000 0.03460 0.02070 = 0.03921 0.00856 0.00484 0.00074 AFIX 43 H13 2 -0.165187 -0.679497 0.286279 11.00000 -1.20000 AFIX 0 C14 1 0.002237 -0.557665 0.201463 11.00000 0.04613 0.02096 = 0.03222 -0.00260 0.00607 0.00906 AFIX 43 H14 2 0.006114 -0.646427 0.156238 11.00000 -1.20000 AFIX 0 C15 1 0.097023 -0.409759 0.188138 11.00000 0.03037 0.02623 = 0.02323 -0.00202 0.00790 0.00853 AFIX 43 H15 2 0.163463 -0.397329 0.133050 11.00000 -1.20000 AFIX 0 C16 1 0.612081 -0.075659 0.282025 11.00000 0.02637 0.03994 = 0.01978 0.00148 0.01132 0.01468 AFIX 137 H16A 2 0.502050 -0.166847 0.258187 11.00000 -1.50000 H16B 2 0.715209 -0.109635 0.301555 11.00000 -1.50000 H16C 2 0.605880 -0.018574 0.210099 11.00000 -1.50000 MOLE 0 AFIX 0 HKLF 4 REM n13065: P-1 REM R1 = 0.0275 for 5508 Fo > 4sig(Fo) and 0.0367 for all 6292 data REM 175 parameters refined using 0 restraints END WGHT 0.0147 0.6604 REM Instructions for potential hydrogen bonds REM No hydrogen bonds found for HTAB generation REM Highest difference peak 1.276, deepest hole -1.363, 1-sigma level 0.200 Q1 1 0.4794 0.1404 0.4699 11.00000 0.05 1.28 Q2 1 0.4594 0.1971 0.4519 11.00000 0.05 1.19 Q3 1 0.2205 0.0706 0.3240 11.00000 0.05 1.15 Q4 1 0.3607 0.1931 0.4223 11.00000 0.05 1.11 Q5 1 0.3347 0.1160 0.4751 11.00000 0.05 1.10 Q6 1 0.2258 0.0590 0.3914 11.00000 0.05 1.10 Q7 1 0.4585 0.0625 0.3837 11.00000 0.05 1.08 Q8 1 0.2369 -0.4264 0.0326 11.00000 0.05 1.05 Q9 1 0.2745 0.0237 0.4452 11.00000 0.05 1.05 Q10 1 0.4653 0.0604 0.4661 11.00000 0.05 1.05 Q11 1 0.2302 -0.0173 0.3513 11.00000 0.05 1.02 Q12 1 0.3376 0.1106 0.3026 11.00000 0.05 0.98 Q13 1 0.3709 -0.0146 0.3823 11.00000 0.05 0.97 Q14 1 0.3031 -0.0339 0.4117 11.00000 0.05 0.96 Q15 1 0.4302 0.2644 0.2423 11.00000 0.05 0.91 Q16 1 0.4076 0.1539 0.3345 11.00000 0.05 0.89 Q17 1 0.3912 0.0865 0.4278 11.00000 0.05 0.86 Q18 1 0.3503 0.1795 0.3540 11.00000 0.05 0.81 Q19 1 0.3468 0.0306 0.3008 11.00000 0.05 0.80 Q20 1 0.4126 0.3653 0.1667 11.00000 0.05 0.78 Q21 1 0.2789 0.1620 0.4059 11.00000 0.05 0.77 Q22 1 0.3463 0.2424 0.4850 11.00000 0.05 0.75 Q23 1 0.0428 -0.0171 0.4980 11.00000 0.05 0.74 Q24 1 0.1694 -0.1198 0.1831 11.00000 0.05 0.71 Q25 1 0.6654 0.1012 0.4695 11.00000 0.05 0.69 Q26 1 0.6328 0.1022 0.3823 11.00000 0.05 0.69 Q27 1 -0.0909 -0.6242 0.3015 11.00000 0.05 0.69 Q28 1 0.5400 0.0889 0.3584 11.00000 0.05 0.69 Q29 1 0.3628 0.0692 0.4859 11.00000 0.05 0.68 Q30 1 0.0046 -0.7537 0.2071 11.00000 0.05 0.68 ; _shelx_res_checksum 72576 _shelx_hkl_file ; -1 0 0 -0.25 0.12 -1 0 0 -0.18 0.13 1 0 0 -0.06 0.13 1 0 0 0.08 0.17 1 0 0 0.02 0.12 -2 0 0 27.89 1.07 -2 0 0 27.55 1.36 -2 0 0 28.13 1.14 2 0 0 28.24 1.15 2 0 0 26.91 1.26 2 0 0 28.00 1.39 2 0 0 28.72 1.07 -3 0 0 420.23 11.96 3 0 0 420.01 13.09 3 0 0 415.00 11.96 -4 0 0 338.08 9.96 4 0 0 341.38 10.95 4 0 0 341.19 9.97 -5 0 0 2.86 0.81 5 0 0 2.19 1.09 5 0 0 3.21 0.83 -6 0 0 108.34 4.00 6 0 0 118.57 4.52 6 0 0 110.44 4.02 6 0 0 118.86 4.92 -7 0 0 162.88 5.65 7 0 0 157.73 5.62 7 0 0 162.75 6.18 7 0 0 155.56 6.52 -8 0 0 34.90 2.30 8 0 0 37.99 3.55 8 0 0 39.02 2.27 8 0 0 31.69 2.27 -9 0 0 26.07 2.60 9 0 0 20.22 2.39 9 0 0 21.32 2.81 -10 0 0 38.78 3.02 10 0 0 42.56 4.50 -11 0 0 31.15 3.52 11 0 0 25.79 3.31 11 0 0 26.58 4.37 12 -1 0 2.55 1.88 11 -1 0 4.41 2.58 11 -1 0 3.64 2.28 -11 1 0 3.03 2.23 10 -1 0 48.34 3.63 10 -1 0 53.31 4.74 -10 1 0 50.50 3.70 9 -1 0 46.76 4.39 9 -1 0 52.91 3.31 -9 1 0 54.40 3.33 8 -1 0 0.97 1.27 8 -1 0 0.11 0.95 8 -1 0 1.74 1.92 -8 1 0 0.06 1.28 7 -1 0 116.84 4.76 7 -1 0 112.78 4.89 7 -1 0 109.13 4.24 -7 1 0 112.61 4.25 6 -1 0 207.70 7.32 6 -1 0 201.00 6.39 -6 1 0 197.28 6.38 5 -1 0 16.81 1.49 5 -1 0 16.36 1.28 -5 1 0 18.81 1.30 4 -1 0 65.12 2.34 4 -1 0 62.15 2.85 -4 1 0 64.23 2.33 3 -1 0 387.96 10.82 3 -1 0 370.59 11.92 -3 1 0 377.81 10.82 2 -1 0 956.71 28.98 2 -1 0 957.60 26.65 2 -1 0 946.31 26.64 -2 1 0 908.60 28.97 -2 1 0 1000.00 26.66 -2 1 0 973.64 26.65 0 -1 0 -0.27 0.15 0 -1 0 -0.22 0.05 0 -1 0 -0.22 0.14 0 -1 0 -0.41 0.13 0 -1 0 -0.20 0.06 0 -1 0 0.04 0.11 0 -1 0 -0.19 0.07 0 1 0 -0.30 0.08 0 1 0 -0.47 0.15 0 1 0 -0.12 0.14 0 1 0 -0.15 0.13 0 1 0 -0.15 0.06 -1 -1 0 815.83 24.47 -1 -1 0 831.64 22.62 -1 -1 0 826.67 25.17 -1 -1 0 800.76 22.61 1 1 0 791.82 22.61 1 1 0 828.10 22.62 1 1 0 810.16 24.47 1 1 0 793.55 25.15 -2 -1 0 8.80 0.91 -2 -1 0 9.59 0.64 2 1 0 8.61 0.63 2 1 0 8.55 0.60 2 1 0 9.08 0.92 -3 -1 0 185.34 5.47 -3 -1 0 180.28 6.17 3 1 0 176.45 5.97 3 1 0 178.50 5.43 -4 -1 0 327.56 9.75 4 1 0 322.71 9.75 4 1 0 341.33 11.45 4 1 0 328.08 10.67 -5 -1 0 83.11 3.09 5 1 0 81.10 3.70 5 1 0 90.23 3.34 5 1 0 81.45 3.09 -6 -1 0 37.90 2.21 6 1 0 41.72 2.26 6 1 0 36.50 1.85 6 1 0 36.64 2.79 -7 -1 0 124.50 4.83 7 1 0 125.10 5.74 7 1 0 132.81 5.02 7 1 0 126.44 4.89 -8 -1 0 58.76 3.36 8 1 0 52.92 3.31 8 1 0 62.67 4.33 -9 -1 0 2.19 1.83 9 1 0 1.05 2.59 9 1 0 0.67 1.85 -10 -1 0 61.02 4.28 10 1 0 52.90 4.59 10 1 0 60.57 4.34 -11 -1 0 28.12 3.43 11 1 0 28.31 3.77 11 1 0 30.99 3.02 11 1 0 29.70 4.56 12 -2 0 9.40 2.15 -12 2 0 16.55 3.05 11 -2 0 2.26 3.16 11 -2 0 0.41 1.99 -11 2 0 0.92 2.09 10 -2 0 15.43 2.70 -10 2 0 17.93 2.35 9 -2 0 84.56 4.09 9 -2 0 68.31 4.26 9 -2 0 69.62 3.69 -9 2 0 69.39 3.69 8 -2 0 30.57 2.71 8 -2 0 34.10 2.08 8 -2 0 35.72 2.59 -8 2 0 33.03 2.06 7 -2 0 38.30 2.97 7 -2 0 38.27 2.17 -7 2 0 34.54 2.13 6 -2 0 89.46 4.02 6 -2 0 85.99 3.21 -6 2 0 83.37 3.19 5 -2 0 91.03 3.82 5 -2 0 91.48 3.11 -5 2 0 85.31 3.08 4 -2 0 4.00 0.62 4 -2 0 4.73 1.06 -4 2 0 3.31 0.60 3 -2 0 214.96 6.14 3 -2 0 203.65 6.97 -3 2 0 210.37 6.14 -3 2 0 212.42 6.15 -3 2 0 214.22 7.05 2 -2 0 334.05 9.49 2 -2 0 333.36 10.15 2 -2 0 342.43 10.57 2 -2 0 322.11 10.45 2 -2 0 331.45 10.79 2 -2 0 346.34 9.49 -2 2 0 338.64 10.57 -2 2 0 345.31 10.78 -2 2 0 343.49 9.49 -2 2 0 330.78 10.49 -2 2 0 343.17 9.50 1 -2 0 114.63 3.83 1 -2 0 116.74 3.64 1 -2 0 114.53 3.28 1 -2 0 114.04 3.96 1 -2 0 118.46 3.28 -1 2 0 120.94 3.86 -1 2 0 122.30 3.28 -1 2 0 118.27 3.97 -1 2 0 120.54 3.28 -1 2 0 114.02 3.65 0 -2 0 178.96 5.83 0 -2 0 181.16 6.00 0 -2 0 170.46 5.78 0 -2 0 173.68 5.02 0 -2 0 179.31 5.02 0 -2 0 177.32 5.64 0 -2 0 173.12 5.44 0 2 0 176.80 5.63 0 2 0 187.70 5.99 0 2 0 181.82 5.82 0 2 0 179.03 5.02 0 2 0 175.49 5.46 -1 -2 0 381.57 12.58 -1 -2 0 399.99 12.66 -1 -2 0 403.70 11.23 -1 -2 0 414.57 12.21 1 2 0 396.00 12.21 1 2 0 404.09 12.02 1 2 0 406.20 11.24 1 2 0 361.29 13.30 1 2 0 396.15 12.24 1 2 0 417.07 11.24 -2 -2 0 74.80 2.99 -2 -2 0 77.35 2.45 2 2 0 74.49 2.72 2 2 0 74.78 2.45 2 2 0 74.60 2.72 2 2 0 75.06 3.02 -3 -2 0 17.46 1.59 -3 -2 0 17.61 1.03 3 2 0 19.72 1.06 3 2 0 17.99 1.41 3 2 0 19.53 0.79 -4 -2 0 296.91 10.43 -4 -2 0 317.23 9.30 4 2 0 323.08 10.71 4 2 0 307.82 9.30 4 2 0 310.13 10.22 -5 -2 0 134.74 4.60 5 2 0 126.73 5.20 5 2 0 136.20 4.81 5 2 0 131.78 4.59 -6 -2 0 0.20 0.74 6 2 0 1.08 1.13 6 2 0 1.44 0.53 6 2 0 -0.18 0.73 -7 -2 0 45.55 2.86 7 2 0 49.89 2.93 7 2 0 49.19 3.67 -8 -2 0 101.45 4.36 8 2 0 106.98 5.80 8 2 0 103.25 4.70 -9 -2 0 18.17 2.58 9 2 0 17.39 2.55 9 2 0 20.37 3.48 9 2 0 22.32 2.92 -10 -2 0 15.43 2.28 10 2 0 16.81 2.31 10 2 0 16.30 3.24 10 2 0 14.91 3.76 -11 -2 0 27.40 3.54 11 2 0 25.09 3.32 12 -3 0 13.05 4.07 -12 3 0 18.30 2.53 11 -3 0 17.08 2.51 11 -3 0 21.99 3.86 -11 3 0 21.71 2.72 10 -3 0 0.15 1.64 10 -3 0 1.52 2.40 -10 3 0 1.07 1.24 9 -3 0 47.51 4.06 9 -3 0 43.84 2.89 9 -3 0 43.67 2.88 -9 3 0 42.63 2.92 -9 3 0 46.00 2.91 8 -3 0 60.08 3.93 8 -3 0 60.99 3.00 8 -3 0 62.12 3.28 -8 3 0 59.34 2.97 -8 3 0 61.32 3.23 7 -3 0 1.62 0.90 7 -3 0 1.01 1.44 -7 3 0 0.01 0.86 -7 3 0 0.87 1.04 6 -3 0 43.45 2.57 6 -3 0 44.44 2.03 -6 3 0 46.35 2.45 -6 3 0 46.21 2.04 5 -3 0 108.43 4.45 5 -3 0 112.62 3.63 -5 3 0 116.40 4.33 -5 3 0 106.41 3.61 4 -3 0 77.19 2.48 4 -3 0 73.34 3.25 -4 3 0 76.32 2.48 -4 3 0 76.20 2.53 -4 3 0 77.31 3.06 3 -3 0 66.47 2.10 3 -3 0 69.23 2.83 -3 3 0 68.11 2.14 -3 3 0 65.02 2.11 -3 3 0 67.58 2.67 2 -3 0 237.82 7.63 2 -3 0 235.98 6.67 -2 3 0 229.33 7.27 -2 3 0 232.90 7.62 -2 3 0 238.92 7.79 -2 3 0 248.49 6.67 -1 3 0 116.37 3.73 -1 3 0 116.40 4.09 -1 3 0 114.62 3.95 0 -3 0 4.47 0.41 0 -3 0 4.47 0.37 0 -3 0 4.80 0.57 0 -3 0 4.80 0.53 0 -3 0 6.62 0.88 0 3 0 4.83 0.81 0 3 0 5.89 0.56 0 3 0 4.48 0.59 0 3 0 3.92 0.38 0 3 0 6.29 0.59 -1 -3 0 297.58 9.83 -1 -3 0 289.46 10.24 -1 -3 0 300.96 8.59 -1 -3 0 316.48 10.27 1 3 0 302.89 9.29 1 3 0 296.67 9.46 1 3 0 290.70 9.42 1 3 0 304.74 8.61 1 3 0 298.80 10.19 1 3 0 312.50 8.62 -2 -3 0 318.72 10.69 -2 -3 0 331.11 9.37 2 3 0 331.74 10.10 2 3 0 323.71 10.21 2 3 0 321.24 9.38 2 3 0 315.49 10.22 -3 -3 0 11.80 1.44 -3 -3 0 11.86 1.00 3 3 0 12.20 1.07 3 3 0 11.20 1.20 3 3 0 11.82 1.24 3 3 0 11.33 1.02 -4 -3 0 60.69 2.43 -4 -3 0 54.87 2.80 4 3 0 55.91 2.69 4 3 0 54.98 2.39 4 3 0 59.35 2.86 -5 -3 0 115.08 4.15 -5 -3 0 116.59 4.82 5 3 0 110.24 4.53 5 3 0 108.61 4.73 5 3 0 115.28 4.16 -6 -3 0 38.24 2.17 6 3 0 38.65 2.20 6 3 0 39.73 3.09 6 3 0 36.66 2.86 -7 -3 0 0.67 1.36 7 3 0 2.73 1.98 7 3 0 1.69 1.33 7 3 0 3.72 1.44 -8 -3 0 57.88 3.70 8 3 0 61.96 3.80 8 3 0 65.09 4.41 8 3 0 62.66 4.82 -9 -3 0 38.49 3.00 9 3 0 44.24 4.12 9 3 0 40.39 4.01 -10 -3 0 -0.04 2.37 10 3 0 0.79 2.06 10 3 0 -2.45 3.26 10 3 0 -3.38 2.36 12 -4 0 6.84 3.71 -12 4 0 4.68 2.41 11 -4 0 34.05 3.70 11 -4 0 35.35 4.32 -11 4 0 38.02 2.81 10 -4 0 17.03 2.11 10 -4 0 19.73 2.64 10 -4 0 15.59 3.15 -10 4 0 17.66 2.15 9 -4 0 12.36 1.67 9 -4 0 9.71 1.69 9 -4 0 7.81 1.90 -9 4 0 10.01 1.69 -9 4 0 11.07 1.78 8 -4 0 67.28 3.10 8 -4 0 77.09 4.27 -8 4 0 67.62 3.49 -8 4 0 67.26 3.09 7 -4 0 54.21 2.42 7 -4 0 54.21 3.40 -7 4 0 51.42 2.39 -7 4 0 54.27 2.92 6 -4 0 1.32 0.64 6 -4 0 1.51 1.24 -6 4 0 1.98 0.67 -6 4 0 1.58 1.00 5 -4 0 117.30 4.70 5 -4 0 121.30 3.73 -5 4 0 115.97 3.72 -5 4 0 113.90 4.45 4 -4 0 230.84 7.88 4 -4 0 232.49 6.76 -4 4 0 233.02 7.98 -4 4 0 241.03 6.82 -4 4 0 229.07 6.76 3 -4 0 6.81 0.44 3 -4 0 8.65 1.15 -3 4 0 6.92 1.03 -3 4 0 7.52 1.08 -3 4 0 7.21 0.47 2 -4 0 75.61 2.94 -2 4 0 77.62 2.92 -2 4 0 75.69 2.65 1 -4 0 290.50 9.42 -1 4 0 269.18 9.17 -1 4 0 270.70 8.88 0 -4 0 162.50 5.62 0 -4 0 156.48 4.60 0 -4 0 154.56 5.58 0 4 0 172.91 5.61 0 4 0 160.76 5.65 0 4 0 160.14 5.20 0 4 0 158.01 5.38 0 4 0 155.33 4.61 -1 -4 0 38.59 1.47 -1 -4 0 35.35 1.35 -1 -4 0 33.07 1.77 -1 -4 0 34.91 2.08 1 4 0 38.54 1.42 1 4 0 35.32 1.37 1 4 0 36.13 1.65 1 4 0 37.00 1.78 -2 -4 0 229.65 6.66 -2 -4 0 221.51 7.81 2 4 0 222.36 7.38 2 4 0 218.70 7.27 2 4 0 223.78 7.33 2 4 0 222.74 6.64 -3 -4 0 67.82 2.54 -3 -4 0 63.83 3.27 3 4 0 68.87 2.56 3 4 0 64.56 2.96 3 4 0 68.05 2.75 3 4 0 66.78 2.91 -4 -4 0 1.74 0.81 -4 -4 0 0.61 1.21 4 4 0 1.43 0.86 4 4 0 1.07 1.08 4 4 0 2.01 0.80 4 4 0 1.49 1.14 -5 -4 0 34.28 2.91 -5 -4 0 32.38 2.15 5 4 0 32.74 2.54 5 4 0 34.78 2.20 5 4 0 32.18 2.71 5 4 0 33.63 1.94 -6 -4 0 60.04 2.86 -6 -4 0 61.57 4.06 6 4 0 57.20 2.82 6 4 0 60.16 3.88 6 4 0 60.27 2.92 6 4 0 56.33 3.65 -7 -4 0 13.64 1.95 7 4 0 13.48 2.45 7 4 0 11.96 2.59 7 4 0 8.93 1.85 -8 -4 0 12.12 2.13 8 4 0 11.71 2.49 8 4 0 10.72 2.74 8 4 0 13.90 2.35 -9 -4 0 22.89 2.49 9 4 0 25.33 3.08 9 4 0 31.60 4.31 9 4 0 31.19 3.29 -10 -4 0 5.60 2.57 12 -5 0 -0.87 2.28 12 -5 0 0.29 2.15 -12 5 0 -2.17 1.96 11 -5 0 42.74 4.55 11 -5 0 41.05 4.03 -11 5 0 39.52 3.32 10 -5 0 42.59 3.81 10 -5 0 49.56 4.40 -10 5 0 42.47 3.00 9 -5 0 2.60 1.76 9 -5 0 0.99 1.60 -9 5 0 4.04 1.55 -9 5 0 2.96 1.29 8 -5 0 50.12 3.75 -8 5 0 45.61 2.49 -8 5 0 49.90 3.01 7 -5 0 141.46 5.91 7 -5 0 142.25 4.66 -7 5 0 135.14 4.64 -7 5 0 139.91 5.54 6 -5 0 52.47 2.09 6 -5 0 52.41 3.20 -6 5 0 56.64 2.87 -6 5 0 53.34 2.12 5 -5 0 32.87 2.35 -5 5 0 29.53 1.35 -5 5 0 31.74 2.09 -5 5 0 31.39 1.37 4 -5 0 157.22 5.72 4 -5 0 155.20 4.54 -4 5 0 153.63 4.54 -4 5 0 161.12 5.67 -4 5 0 149.61 5.68 -4 5 0 154.52 4.58 3 -5 0 168.40 6.06 3 -5 0 179.03 4.92 -3 5 0 182.15 4.97 -3 5 0 176.42 4.92 -3 5 0 172.45 6.10 -3 5 0 164.69 5.67 -2 5 0 1.73 0.64 -2 5 0 0.26 0.57 -2 5 0 0.97 0.64 1 -5 0 188.13 5.18 1 -5 0 189.61 6.52 1 -5 0 173.93 5.19 1 -5 0 185.10 6.53 -1 5 0 183.68 6.31 -1 5 0 187.51 6.04 -1 5 0 189.34 6.55 -1 5 0 189.25 5.18 -1 5 0 185.81 5.20 0 -5 0 303.93 10.48 0 -5 0 321.01 10.75 0 -5 0 334.78 11.03 0 -5 0 322.68 8.91 0 5 0 301.44 10.49 0 5 0 312.81 8.90 0 5 0 303.80 9.82 0 5 0 310.96 10.12 -1 -5 0 15.57 1.41 -1 -5 0 13.55 0.82 -1 -5 0 14.36 1.20 -1 -5 0 16.32 0.88 1 5 0 15.36 0.87 1 5 0 12.14 0.97 1 5 0 14.81 1.33 1 5 0 14.49 1.30 -2 -5 0 59.56 2.99 -2 -5 0 63.45 2.32 2 5 0 62.60 2.33 2 5 0 68.95 2.84 2 5 0 62.56 2.70 -3 -5 0 86.82 3.05 -3 -5 0 79.15 3.93 3 5 0 81.44 3.61 3 5 0 77.52 3.51 3 5 0 82.41 3.05 3 5 0 85.82 3.35 -4 -5 0 25.02 2.22 -4 -5 0 23.49 1.75 4 5 0 23.62 1.94 4 5 0 23.21 2.16 4 5 0 24.13 1.74 4 5 0 23.91 1.80 -5 -5 0 6.13 1.58 -5 -5 0 4.47 1.25 5 5 0 4.20 1.24 5 5 0 2.64 1.33 5 5 0 4.55 1.34 5 5 0 2.25 0.96 -6 -5 0 65.62 4.44 -6 -5 0 63.89 3.37 6 5 0 62.56 3.38 6 5 0 66.97 4.32 6 5 0 64.17 4.04 -7 -5 0 22.18 2.37 7 5 0 26.14 2.52 7 5 0 23.15 3.28 7 5 0 22.88 2.61 -8 -5 0 0.15 1.26 8 5 0 0.54 2.51 8 5 0 0.30 1.99 8 5 0 2.17 1.40 9 5 0 12.01 3.52 9 5 0 11.55 2.84 12 -6 0 1.59 3.20 12 -6 0 2.18 2.47 -12 6 0 2.18 2.07 11 -6 0 25.18 3.34 11 -6 0 23.00 3.21 -11 6 0 29.04 2.69 10 -6 0 48.69 3.59 10 -6 0 53.22 4.72 -10 6 0 54.75 3.13 -10 6 0 52.25 3.62 9 -6 0 38.19 3.33 9 -6 0 39.14 3.51 -9 6 0 38.40 3.04 -9 6 0 39.33 2.47 8 -6 0 7.08 1.70 -8 6 0 7.38 1.22 -8 6 0 6.86 1.62 7 -6 0 131.01 5.58 -7 6 0 132.45 4.35 -7 6 0 130.92 5.28 6 -6 0 88.82 4.22 -6 6 0 87.47 3.93 -6 6 0 82.91 2.88 5 -6 0 5.60 0.53 5 -6 0 5.57 1.21 -5 6 0 5.51 0.62 -5 6 0 6.67 0.57 -5 6 0 5.94 1.29 4 -6 0 106.09 4.32 4 -6 0 106.40 3.07 -4 6 0 105.81 3.07 -4 6 0 107.43 3.15 -4 6 0 95.83 4.13 3 -6 0 223.61 7.69 -3 6 0 233.63 7.37 -3 6 0 225.31 7.97 -3 6 0 225.52 7.83 2 -6 0 57.55 2.40 -2 6 0 54.93 2.70 -2 6 0 57.12 2.86 -2 6 0 54.71 2.37 1 -6 0 33.61 1.72 1 -6 0 33.52 2.19 1 -6 0 34.99 1.04 -1 6 0 31.79 1.82 -1 6 0 38.22 1.08 -1 6 0 34.73 2.05 -1 6 0 35.40 1.04 -1 6 0 32.06 2.02 0 -6 0 306.72 8.59 0 -6 0 300.49 10.45 0 -6 0 292.64 10.32 0 -6 0 314.96 10.69 0 6 0 294.59 9.61 0 6 0 294.57 10.37 0 6 0 303.77 8.59 -1 -6 0 60.44 2.84 -1 -6 0 62.11 2.18 -1 -6 0 60.45 3.24 -1 -6 0 67.76 2.55 1 6 0 63.62 2.84 1 6 0 58.09 2.77 1 6 0 65.18 2.20 -2 -6 0 5.28 0.75 -2 -6 0 7.76 1.60 2 6 0 6.43 0.83 2 6 0 6.32 1.13 2 6 0 5.09 1.19 -3 -6 0 94.66 3.45 -3 -6 0 96.01 4.63 3 6 0 94.49 3.45 3 6 0 97.87 3.86 3 6 0 85.34 3.83 -4 -6 0 101.99 3.79 -4 -6 0 103.62 5.16 4 6 0 104.30 4.16 4 6 0 97.85 3.77 4 6 0 107.73 4.84 4 6 0 106.31 4.45 -5 -6 0 2.96 2.17 -5 -6 0 2.21 0.92 5 6 0 4.28 1.32 5 6 0 0.89 1.28 5 6 0 1.31 1.75 5 6 0 2.59 1.07 -6 -6 0 23.80 3.31 6 6 0 22.38 3.14 6 6 0 29.94 3.14 7 6 0 38.51 2.88 7 6 0 38.58 4.17 7 6 0 46.68 4.11 8 6 0 12.36 2.50 8 6 0 9.34 3.41 8 6 0 7.24 2.95 12 -7 0 6.97 2.55 12 -7 0 8.66 3.01 -12 7 0 7.58 2.10 11 -7 0 -0.09 2.32 11 -7 0 2.67 2.98 -11 7 0 0.97 1.59 10 -7 0 60.38 4.62 10 -7 0 61.82 4.32 -10 7 0 61.66 3.21 -10 7 0 63.02 4.01 9 -7 0 52.15 4.17 9 -7 0 63.34 4.69 -9 7 0 56.80 3.69 -9 7 0 60.51 2.83 8 -7 0 1.64 1.95 -8 7 0 2.27 0.90 -8 7 0 4.28 1.56 7 -7 0 71.47 3.86 -7 7 0 69.45 2.58 -7 7 0 70.81 3.78 6 -7 0 139.65 5.90 -6 7 0 141.33 5.79 -6 7 0 141.64 4.34 5 -7 0 24.49 2.00 -5 7 0 23.49 0.93 -5 7 0 26.04 2.33 4 -7 0 28.50 1.94 -4 7 0 26.13 2.25 -4 7 0 27.35 1.60 -4 7 0 28.22 2.02 3 -7 0 211.20 7.43 3 -7 0 223.08 7.70 -3 7 0 215.60 7.06 -3 7 0 200.59 7.43 -3 7 0 207.07 7.77 2 -7 0 216.66 7.55 2 -7 0 209.33 7.61 -2 7 0 211.52 7.00 -2 7 0 201.53 7.61 -2 7 0 210.29 7.35 1 -7 0 12.57 1.33 1 -7 0 12.62 1.65 1 -7 0 13.12 1.29 -1 7 0 11.67 1.32 -1 7 0 11.11 1.68 0 -7 0 95.45 4.40 0 -7 0 98.57 3.99 0 -7 0 100.54 3.04 0 -7 0 100.55 4.00 0 7 0 96.04 3.78 0 7 0 101.36 4.09 0 7 0 94.19 4.40 0 7 0 97.21 3.02 -1 -7 0 203.73 7.68 -1 -7 0 192.21 7.43 1 7 0 213.94 6.09 1 7 0 191.46 6.90 1 7 0 205.53 7.14 -2 -7 0 16.15 2.21 2 7 0 15.11 1.63 2 7 0 17.41 1.88 -3 -7 0 49.04 3.76 3 7 0 58.48 2.96 3 7 0 59.64 3.36 -4 -7 0 106.46 5.63 4 7 0 105.47 4.96 4 7 0 106.58 4.44 -5 -7 0 47.50 4.23 5 7 0 50.46 3.82 5 7 0 38.83 2.82 -6 -7 0 -0.25 1.83 6 7 0 2.07 1.73 6 7 0 3.40 2.34 7 7 0 31.74 2.97 7 7 0 30.52 3.80 12 -8 0 19.31 4.27 12 -8 0 28.39 3.32 -12 8 0 26.62 2.57 11 -8 0 2.14 2.53 11 -8 0 2.90 2.31 -11 8 0 2.71 1.51 10 -8 0 23.48 2.84 10 -8 0 21.31 3.51 -10 8 0 16.75 1.76 -10 8 0 20.08 2.68 9 -8 0 65.49 4.75 9 -8 0 76.46 5.13 -9 8 0 67.02 3.12 -9 8 0 73.63 4.30 8 -8 0 30.64 3.29 8 -8 0 31.22 3.13 -8 8 0 25.22 1.75 -8 8 0 23.49 2.34 7 -8 0 26.18 2.89 -7 8 0 22.32 1.22 6 -8 0 121.24 5.40 -6 8 0 113.21 3.43 -6 8 0 107.05 5.18 5 -8 0 88.53 4.38 -5 8 0 88.73 4.43 -5 8 0 97.29 4.52 4 -8 0 3.99 1.38 -4 8 0 4.21 1.56 -4 8 0 3.33 1.44 -4 8 0 5.79 1.19 3 -8 0 155.57 6.00 3 -8 0 160.73 6.06 -3 8 0 156.86 6.06 -3 8 0 164.21 5.71 -3 8 0 156.31 6.25 2 -8 0 123.32 5.18 2 -8 0 122.97 5.05 2 -8 0 126.65 4.84 -2 8 0 122.79 4.65 -2 8 0 122.41 5.05 -2 8 0 117.01 5.12 1 -8 0 39.48 2.80 1 -8 0 37.37 2.26 1 -8 0 40.14 2.14 -1 8 0 34.82 2.25 -1 8 0 34.01 2.81 0 -8 0 55.48 3.10 0 -8 0 52.36 2.69 0 8 0 48.37 2.70 0 8 0 52.75 2.83 0 8 0 53.58 1.81 -1 -8 0 144.07 5.98 -1 -8 0 152.95 6.50 1 8 0 151.95 4.75 1 8 0 159.34 5.94 1 8 0 159.65 5.90 -2 -8 0 69.57 4.40 2 8 0 75.64 2.85 2 8 0 74.53 3.88 -3 -8 0 0.26 1.93 3 8 0 1.42 1.20 3 8 0 1.27 0.98 3 8 0 1.65 1.73 -4 -8 0 57.62 4.12 4 8 0 65.70 3.15 4 8 0 71.08 4.18 4 8 0 55.90 3.62 -5 -8 0 43.00 4.36 5 8 0 47.19 3.06 5 8 0 42.18 4.03 -6 -8 0 -3.88 2.78 6 8 0 -1.90 2.48 6 8 0 3.98 1.90 7 8 0 12.28 3.36 7 8 0 13.12 2.47 12 -9 0 19.69 3.02 11 -9 0 12.75 3.58 11 -9 0 13.47 3.08 -11 9 0 12.64 1.78 10 -9 0 5.19 2.96 10 -9 0 0.12 2.31 -10 9 0 0.96 1.05 -10 9 0 3.68 2.04 9 -9 0 41.49 3.51 9 -9 0 43.55 4.19 -9 9 0 38.50 3.09 -9 9 0 38.81 2.00 8 -9 0 49.06 4.27 8 -9 0 44.63 3.96 -8 9 0 47.00 3.80 7 -9 0 2.10 1.48 7 -9 0 4.25 1.95 -7 9 0 5.34 1.93 6 -9 0 48.38 3.70 -6 9 0 50.67 3.25 5 -9 0 125.33 5.43 -5 9 0 114.14 5.47 -5 9 0 115.89 5.56 4 -9 0 26.61 2.52 4 -9 0 26.99 2.11 4 -9 0 20.86 2.04 -4 9 0 27.14 2.75 -4 9 0 28.38 2.64 -4 9 0 27.96 2.27 3 -9 0 16.15 1.94 3 -9 0 15.19 1.88 3 -9 0 16.92 1.65 3 -9 0 10.99 1.86 -3 9 0 16.87 1.62 -3 9 0 13.10 2.02 -3 9 0 11.10 2.09 2 -9 0 122.15 5.35 2 -9 0 134.68 5.51 2 -9 0 127.14 5.10 -2 9 0 126.71 4.85 -2 9 0 118.91 5.16 -2 9 0 132.58 5.63 1 -9 0 54.12 2.83 1 -9 0 46.78 2.67 1 -9 0 45.65 3.44 -1 9 0 49.60 2.93 -1 9 0 52.84 3.28 -1 9 0 49.45 2.87 0 -9 0 -0.32 1.66 0 9 0 -1.11 1.27 0 9 0 -0.01 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3.07 4 -11 0 47.15 3.73 -4 11 0 49.02 2.93 -4 11 0 45.04 4.07 -4 11 0 52.12 3.70 3 -11 0 37.84 3.58 3 -11 0 35.99 3.08 3 -11 0 36.87 3.33 -3 11 0 43.22 3.75 -3 11 0 42.88 3.12 -3 11 0 38.14 3.47 2 -11 0 1.60 2.01 -2 11 0 2.81 1.97 -2 11 0 3.68 2.43 -2 11 0 2.58 1.66 1 -11 0 40.82 3.95 -1 11 0 45.48 3.42 -1 11 0 46.66 3.75 0 -11 0 46.20 3.68 0 11 0 38.44 3.54 0 11 0 43.49 3.52 -1 -11 0 -0.69 2.49 1 11 0 -1.30 1.77 1 11 0 -0.20 2.08 -2 -11 0 18.07 3.02 2 11 0 18.19 2.43 2 11 0 19.38 2.59 -3 -11 0 26.76 4.21 3 11 0 31.85 3.28 10 -12 0 28.73 4.41 10 -12 0 27.47 4.03 -10 12 0 20.09 3.53 9 -12 0 14.53 2.62 9 -12 0 16.91 3.58 -9 12 0 6.21 2.89 8 -12 0 0.77 2.37 8 -12 0 1.83 2.64 8 -12 0 -0.04 2.41 -8 12 0 0.04 2.61 7 -12 0 29.12 3.23 7 -12 0 31.63 3.77 7 -12 0 33.15 3.60 -7 12 0 34.97 4.02 6 -12 0 37.65 3.93 6 -12 0 24.04 2.90 6 -12 0 35.13 3.56 -6 12 0 31.48 3.92 5 -12 0 4.68 2.19 5 -12 0 2.49 1.38 5 -12 0 2.28 1.92 -5 12 0 2.75 2.48 -5 12 0 1.03 1.77 4 -12 0 29.04 3.09 4 -12 0 21.85 2.89 4 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3.23 7 7 -4 32.02 3.18 6 7 -4 18.69 2.57 6 7 -4 21.81 2.19 6 7 -4 20.90 2.66 5 7 -4 3.20 1.28 5 7 -4 4.35 1.86 5 7 -4 3.30 1.73 -5 -7 4 4.44 2.10 4 7 -4 57.25 2.67 4 7 -4 52.69 3.63 4 7 -4 59.18 3.37 -4 -7 4 60.77 3.84 3 7 -4 40.19 2.63 3 7 -4 37.67 3.01 3 7 -4 36.15 1.91 -3 -7 4 35.43 2.82 2 7 -4 3.01 0.72 2 7 -4 3.77 1.44 -2 -7 4 3.78 0.98 -2 -7 4 1.64 1.30 1 7 -4 89.40 3.55 1 7 -4 85.48 4.22 1 7 -4 93.19 3.00 -1 -7 4 83.00 4.03 -1 -7 4 83.54 3.81 0 7 -4 133.28 4.93 0 7 -4 127.26 4.05 0 7 -4 133.74 5.46 0 -7 4 137.18 5.65 0 -7 4 132.12 4.50 0 -7 4 129.65 4.96 -1 7 -4 18.69 1.78 -1 7 -4 18.73 1.04 -1 7 -4 21.95 2.12 1 -7 4 20.24 1.75 1 -7 4 22.13 1.53 -2 7 -4 48.21 2.68 -2 7 -4 40.45 1.58 -2 7 -4 47.91 2.38 -2 7 -4 51.85 1.79 2 -7 4 53.80 2.33 2 -7 4 51.24 3.05 -3 7 -4 143.74 5.52 -3 7 -4 144.44 5.76 -3 7 -4 145.01 4.38 3 -7 4 138.95 6.09 3 -7 4 139.71 4.98 3 -7 4 152.31 5.87 -4 7 -4 40.39 1.62 -4 7 -4 38.99 2.79 -4 7 -4 36.58 2.31 4 -7 4 32.92 2.52 4 -7 4 34.83 2.91 -5 7 -4 14.92 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340.94 10.34 2 -3 4 360.17 12.75 2 -3 4 346.94 11.39 2 -3 4 356.88 11.25 2 -3 4 357.62 10.36 -3 3 -4 216.64 6.66 -3 3 -4 223.17 7.09 -3 3 -4 215.39 6.93 3 -3 4 209.79 6.70 3 -3 4 207.38 8.12 3 -3 4 224.24 6.67 3 -3 4 209.32 7.42 -4 3 -4 8.23 0.70 -4 3 -4 10.29 1.15 4 -3 4 9.31 1.32 4 -3 4 6.96 0.66 4 -3 4 8.99 1.38 4 -3 4 10.08 1.15 -5 3 -4 88.51 3.07 -5 3 -4 86.07 3.46 5 -3 4 79.50 3.95 5 -3 4 91.18 4.21 5 -3 4 93.45 3.50 -6 3 -4 133.93 4.84 6 -3 4 119.70 5.65 6 -3 4 127.04 5.69 6 -3 4 134.14 4.82 -7 3 -4 12.33 1.79 7 -3 4 12.22 1.76 7 -3 4 13.58 2.06 7 -3 4 12.78 2.46 -8 3 -4 26.58 2.30 8 -3 4 28.57 2.60 8 -3 4 31.88 3.48 8 -3 4 28.23 2.98 -9 3 -4 49.38 3.78 9 -3 4 50.92 3.75 9 -3 4 57.13 4.16 9 -3 4 46.00 3.33 -10 3 -4 17.84 2.79 10 -3 4 20.46 3.67 10 -3 4 15.57 2.77 11 2 -4 43.67 4.79 11 2 -4 43.04 3.80 -11 -2 4 36.31 3.55 10 2 -4 29.17 3.09 10 2 -4 36.12 3.93 10 2 -4 29.67 2.86 -10 -2 4 31.68 3.08 9 2 -4 3.01 1.75 9 2 -4 0.57 1.44 9 2 -4 2.23 1.34 -9 -2 4 2.33 1.24 8 2 -4 66.82 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67.49 3.12 -6 -4 5 67.78 3.10 5 4 -5 100.72 3.83 5 4 -5 100.39 4.29 5 4 -5 90.57 3.49 -5 -4 5 97.08 3.51 4 4 -5 6.76 1.02 4 4 -5 5.99 0.47 4 4 -5 5.66 0.78 -4 -4 5 4.64 0.75 3 4 -5 73.84 2.83 3 4 -5 75.23 2.72 -3 -4 5 73.74 2.69 2 4 -5 159.69 4.97 2 4 -5 164.34 5.34 -2 -4 5 158.83 4.94 -2 -4 5 155.62 6.30 1 4 -5 16.48 1.49 1 4 -5 13.53 1.20 1 4 -5 13.95 1.03 -1 -4 5 16.99 1.79 -1 -4 5 16.31 1.03 -1 -4 5 16.39 0.68 0 4 -5 115.57 3.68 0 4 -5 109.30 4.40 0 4 -5 115.34 4.03 0 4 -5 117.18 3.67 0 -4 5 115.33 3.70 0 -4 5 112.93 4.17 0 -4 5 112.34 4.82 -1 4 -5 131.30 4.41 -1 4 -5 144.23 5.08 1 -4 5 141.13 4.49 1 -4 5 139.35 5.69 -2 4 -5 45.25 2.06 -2 4 -5 49.24 2.34 2 -4 5 49.91 2.58 2 -4 5 47.75 2.83 -3 4 -5 21.07 1.54 -3 4 -5 18.90 1.28 3 -4 5 21.72 1.75 3 -4 5 21.61 1.79 3 -4 5 20.16 1.33 -4 4 -5 107.56 4.07 -4 4 -5 102.34 3.78 4 -4 5 106.62 4.90 4 -4 5 107.82 3.88 4 -4 5 101.62 4.46 -5 4 -5 27.59 1.80 5 -4 5 31.44 2.07 5 -4 5 30.27 2.89 5 -4 5 30.51 2.28 -6 4 -5 0.40 1.06 6 -4 5 1.86 1.23 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197.32 7.50 1 3 -5 130.22 4.43 1 3 -5 130.69 4.19 -1 -3 5 132.44 4.18 -1 -3 5 129.18 5.49 -1 -3 5 141.55 4.65 0 3 -5 7.10 0.70 0 3 -5 7.59 0.83 0 3 -5 8.72 1.16 0 -3 5 10.63 0.92 0 -3 5 9.52 1.41 -1 3 -5 181.13 6.11 -1 3 -5 176.42 5.61 1 -3 5 179.19 7.09 1 -3 5 178.40 6.15 1 -3 5 186.08 5.67 -2 3 -5 119.91 4.08 -2 3 -5 119.11 4.23 2 -3 5 118.24 4.54 2 -3 5 122.19 4.08 2 -3 5 114.58 4.97 -3 3 -5 1.86 0.87 -3 3 -5 3.84 0.77 3 -3 5 2.68 1.15 3 -3 5 2.44 0.89 3 -3 5 1.26 1.06 -4 3 -5 34.28 1.82 -4 3 -5 29.66 1.78 4 -3 5 31.38 1.80 4 -3 5 33.13 2.56 4 -3 5 29.64 2.38 -5 3 -5 145.73 5.25 5 -3 5 157.26 5.42 5 -3 5 157.04 6.23 5 -3 5 148.01 6.44 -6 3 -5 18.38 1.93 6 -3 5 18.62 2.26 6 -3 5 21.74 2.58 6 -3 5 19.50 1.76 -7 3 -5 13.99 1.71 7 -3 5 18.13 2.74 7 -3 5 15.42 2.22 7 -3 5 12.34 1.66 -8 3 -5 66.79 4.04 8 -3 5 68.75 4.36 8 -3 5 71.77 4.99 8 -3 5 60.25 3.96 -9 3 -5 21.86 2.83 9 -3 5 16.72 2.21 9 -3 5 24.86 3.72 9 -3 5 17.24 2.25 -10 3 -5 1.12 2.37 10 -3 5 1.44 3.17 11 2 -5 39.10 3.31 11 2 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30.52 2.18 0 -5 9 32.94 2.21 0 -5 9 36.61 3.33 -1 5 -9 104.84 4.26 -1 5 -9 115.57 4.74 1 -5 9 109.59 4.84 1 -5 9 104.36 5.68 1 -5 9 110.72 4.32 -2 5 -9 53.32 2.66 -2 5 -9 55.23 2.99 2 -5 9 43.30 3.84 2 -5 9 52.82 3.51 -3 5 -9 9.83 1.48 -3 5 -9 8.13 1.62 3 -5 9 7.77 1.83 3 -5 9 8.53 1.63 3 -5 9 9.64 1.74 -4 5 -9 79.13 3.89 4 -5 9 74.86 3.82 4 -5 9 66.75 4.46 4 -5 9 71.74 4.94 -5 5 -9 37.40 2.70 5 -5 9 39.82 4.15 5 -5 9 44.10 4.09 -6 5 -9 -0.15 1.90 6 -5 9 -1.38 2.22 6 -5 9 -2.86 2.37 -7 5 -9 37.50 3.41 7 -5 9 28.90 3.80 7 -5 9 31.92 3.36 -8 5 -9 19.14 3.09 8 -5 9 14.77 3.26 8 -5 9 17.35 2.90 -11 -4 9 8.77 2.88 10 4 -9 4.91 2.31 -10 -4 9 1.97 2.31 9 4 -9 65.12 3.54 -9 -4 9 55.28 3.42 8 4 -9 62.78 3.67 -8 -4 9 57.41 3.66 7 4 -9 -1.24 1.01 7 4 -9 0.63 0.97 -7 -4 9 2.31 1.52 6 4 -9 65.70 2.96 6 4 -9 63.45 3.24 -6 -4 9 61.36 3.22 5 4 -9 147.22 5.04 5 4 -9 136.37 4.93 -5 -4 9 134.53 4.89 4 4 -9 29.36 1.90 4 4 -9 32.20 1.87 -4 -4 9 33.67 1.88 3 4 -9 69.59 3.04 3 4 -9 68.20 2.91 -3 -4 9 68.82 3.01 2 4 -9 149.28 6.01 2 4 -9 140.49 5.02 -2 -4 9 152.16 5.05 -2 -4 9 147.00 6.85 1 4 -9 81.11 4.00 1 4 -9 84.13 3.54 -1 -4 9 88.90 3.55 -1 -4 9 91.94 4.94 0 4 -9 1.30 1.16 0 4 -9 1.33 1.09 0 -4 9 1.02 1.08 0 -4 9 2.07 1.65 -1 4 -9 95.02 3.91 -1 4 -9 86.70 3.74 1 -4 9 88.33 3.79 1 -4 9 78.97 4.84 1 -4 9 94.83 4.18 -2 4 -9 112.67 4.30 -2 4 -9 105.47 4.31 2 -4 9 109.16 4.61 2 -4 9 98.11 5.52 -3 4 -9 8.94 1.68 -3 4 -9 8.68 1.18 3 -4 9 7.54 1.69 3 -4 9 9.35 1.94 3 -4 9 8.09 2.12 -4 4 -9 49.88 3.33 4 -4 9 50.38 4.19 4 -4 9 56.19 3.81 4 -4 9 49.67 3.34 -5 4 -9 68.77 3.64 5 -4 9 78.46 4.68 5 -4 9 77.85 5.06 5 -4 9 62.25 3.58 -6 4 -9 20.33 2.76 6 -4 9 16.75 3.00 6 -4 9 18.57 2.99 6 -4 9 21.35 2.69 -7 4 -9 4.22 2.27 7 -4 9 1.63 2.47 7 -4 9 5.02 2.72 -8 4 -9 37.24 3.78 8 -4 9 34.75 3.57 11 3 -9 26.16 2.86 -11 -3 9 23.74 2.68 10 3 -9 0.96 2.11 -10 -3 9 -0.76 2.01 9 3 -9 37.49 3.04 -9 -3 9 35.61 3.01 8 3 -9 75.61 3.93 -8 -3 9 79.43 3.99 7 3 -9 40.27 2.40 7 3 -9 34.95 2.20 -7 -3 9 39.58 2.39 6 3 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128.83 4.75 -1 -1 9 126.88 4.73 -1 -1 9 138.56 4.82 -1 -1 9 145.67 6.27 0 1 -9 183.74 6.08 0 1 -9 168.21 6.03 0 -1 9 187.35 7.71 0 -1 9 173.46 6.07 0 -1 9 181.06 6.20 -1 1 -9 6.52 0.84 -1 1 -9 7.93 0.77 -1 1 -9 9.25 1.51 1 -1 9 8.84 1.30 1 -1 9 6.75 1.59 1 -1 9 8.90 1.59 -2 1 -9 29.59 2.49 2 -1 9 27.77 2.50 2 -1 9 34.45 2.67 2 -1 9 27.23 2.29 -3 1 -9 119.71 5.26 3 -1 9 133.37 5.43 3 -1 9 123.54 5.93 3 -1 9 134.02 5.30 -4 1 -9 46.54 3.43 4 -1 9 51.20 3.39 4 -1 9 44.19 3.53 4 -1 9 55.74 3.93 -5 1 -9 7.82 2.28 5 -1 9 9.94 2.15 5 -1 9 6.15 2.18 5 -1 9 7.41 2.22 -6 1 -9 77.38 4.64 6 -1 9 58.46 4.44 6 -1 9 62.53 4.57 6 -1 9 68.30 3.99 -7 1 -9 25.84 3.43 7 -1 9 31.29 3.66 7 -1 9 21.44 3.07 8 -1 9 0.78 1.96 12 0 -9 0.28 1.59 12 0 -9 2.66 2.62 -12 0 9 0.50 1.69 11 0 -9 7.33 2.21 11 0 -9 9.64 2.59 -11 0 9 5.80 2.24 10 0 -9 34.51 3.15 10 0 -9 34.14 2.94 -10 0 9 36.49 3.16 9 0 -9 27.11 2.45 9 0 -9 28.38 2.64 9 0 -9 22.57 2.40 -9 0 9 26.09 2.53 8 0 -9 2.37 1.42 8 0 -9 3.11 1.46 8 0 -9 0.53 1.10 -8 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